WO2012020641A1 - Inner cylinder for pressure container and process for production thereof - Google Patents

Abstract

The purpose of the present invention is to provide: an inner cylinder for a pressure container in which durability can be imparted to a flange and which can be used under supercritical conditions even when a material for coating the inner surface of the pressure container and a material for forming the flange are different from each other; and a process for producing the inner cylinder for a pressure container. This inner cylinder for a pressure container has such a structure that a main body (81) and a lid (91) of a pressure container (901) together form a seal part and tightly seal the inside of the pressure container (901). The cylinder comprises cover parts (86, 96) which cover the inner surface of the pressure container, flange-attaching parts which extend from the entire circumferences of the edge parts of the cover parts toward the centrifugal direction, and ring-shaped flanges (84, 94) which are respectively bonded to the flange-attaching parts (85, 95), wherein the cover parts and the corresponding flange-attaching parts are respectively processed in an integrated manner and comprise platinum or a platinum alloy, the flanges comprise iridium, ruthenium or an alloy containing at least one element selected from iridium and ruthenium, and the bonding is diffusion bonding.

Description

Inner cylinder for pressure vessel and manufacturing method thereof

The present invention relates to an inner cylinder for a pressure vessel used under high-temperature and high-pressure conditions, and more particularly to an inner cylinder for a pressure vessel mainly used for growing a single crystal under supercritical conditions.

In recent years, in chemical reactions such as synthesis, decomposition, and crystal growth, processing using a solvent in a supercritical state is performed for the purpose of improving reaction efficiency, reactivity, and the like. Depending on the type of solvent to be used, for example, a hydrothermal synthesis method using water as a solvent, and an athermal synthesis method using ammonia as a solvent can be given. Such treatment is carried out under supercritical conditions in a pressure vessel called an autoclave. The processing conditions may be implemented, for example, in an ultrahigh temperature and ultrahigh pressure state of 800 ° C. and 4000 atmospheres.

The single crystal synthesized using the pressure vessel is, for example, artificial quartz or zinc oxide in the hydrothermal synthesis method. In the low temperature synthesis method, for example, gallium nitride. These single crystals are used for various applications such as optics and electronic elements, and high purity is required. Therefore, it is required that the portion exposed to the inside of the pressure vessel does not elute impurities in an ultra-high temperature and ultra-high pressure state. Therefore, platinum group metals are often used in the portions that come into contact with the chemical solution and the chemical atmosphere.

However, since platinum group metals are extremely expensive, there are problems such as a very high price when the pressure vessel is formed of a bulk metal, poor workability, and insufficient physical strength. For this reason, normally, the main body is made of a heat-resistant alloy such as a nickel-containing alloy to maintain physical strength, and only a portion exposed to the inside of the pressure vessel is provided with a thin lining made of platinum or a platinum alloy. (For example, see FIG. 1 of Patent Document 1).

In the pressure vessel including FIG. 1 of Patent Document 1, the inside of the pressure vessel is covered with a lining having a flange portion (hereinafter referred to as a flange), and the flange provided inside the main body and the inside of the lid The container is sealed with a ring-shaped gasket interposed between the lining cover and the lining cover. The flange, the gasket, and the lining cover form an airtight seal. Since a large pressure is applied to the hermetic seal portion, the flange, the gasket, and the lining cover are damaged by each other to hold the pressure. If these are greatly deformed, the contact area becomes large and the pressure applied to the hermetic seal portion becomes relatively small. For example, when used under a high pressure condition exceeding 1000 atm, there is a problem that the seal becomes insufficient. It was. In particular, when the flange is deformed, the integrally formed lining needs to be replaced. As described above, since expensive platinum is used, if the frequency of replacement is high, the financial burden becomes large.

Therefore, in FIG. 3 of Patent Document 1, the lining body covering the inner surface of the pressure vessel is made of a material having excellent extensibility such as platinum, and the flange has high surface pressure strength such as iridium and is plastically deformed. There has been proposed a technology that makes it possible to repeatedly use the lining by preventing the deformation of the sealing surface in service by using a difficult material.

Although the use is different, as a method for hardening the surface of the metal, a technique is disclosed in which a coating layer made of nickel or a nickel alloy is formed on the surface of a substrate made of titanium or a titanium alloy and alloyed by melt diffusion ( (For example, see Patent Document 2 or 3.)

JP 2006-193355 A JP-A-5-65622 JP-A-5-156422

FIG. 3 of Patent Document 1 is a method in which a lining body made of platinum and a flange made of iridium are butted together at a joint portion and joined by welding or the like. In this method, although both platinum and iridium are platinum group metals, there is a problem that the welded portion becomes weak because the coefficients of thermal expansion differ greatly.

Patent Documents 2 and 3 propose a method for curing a metal surface. In this method, a boundary portion between a base material made of titanium or a titanium alloy and a coating layer made of nickel or a nickel alloy is set as a eutectic point. It is a method in which the surface can be cured by heating to the above temperature and melting and diffusing to cause hardening by eutectic alloying, not a method of curing the surface of platinum or a platinum alloy.

An object of the present invention is to solve the above-described problems, and includes a material that prevents deformation of the flange, imparts durability, and covers the inner surface of the pressure vessel and a material that forms the flange. An object of the present invention is to provide an inner cylinder for a pressure vessel that can withstand use under supercritical conditions even if it is made of different materials, and a method for manufacturing the same.

As a result of intensive studies, the present inventors have coated the inner surface of the pressure vessel with a material excellent in corrosion resistance and workability, and the flange that forms a seal portion for sealing the pressure vessel has excellent corrosion resistance and high surface hardness. The inventors have found that the above problem can be solved by forming them with a material that is not easily deformed, integrating them by diffusion bonding, and increasing the bonding area to bond them more firmly. That is, an inner cylinder for a pressure vessel according to the present invention has a structure in which the pressure vessel forms a seal portion with at least a bottomed cylindrical main body and a lid and seals the inside, and the inside of the pressure vessel A covering portion covering the surface, a flange mounting portion extending in the centrifugal direction over the entire periphery from the end portion of the covering portion, and an annular shape that is joined to the flange mounting portion and serves as a sealing portion of the seal portion A flange for a pressure vessel, wherein the covering portion and the flange mounting portion are integrally processed and made of platinum or a platinum alloy, and the flange is made of iridium, ruthenium, iridium, or ruthenium. And the joining is a diffusion joining in which a metal element contained in the flange and a metal element contained in the flange mounting portion are diffused. .

In the inner tube for a pressure vessel according to the present invention, it is preferable that the surface of the seal portion of the flange has a Vickers hardness of 350 Hv or more measured according to JIS Z 2244: 2009. The deformation of the flange can be prevented and the life of the pressure vessel can be kept longer.

In the inner tube for a pressure vessel according to the present invention, the flange has an outer peripheral surface, the flange mounting portion has a peripheral wall portion processed integrally with the flange mounting portion, and the outer peripheral surface of the flange. It is preferable that the peripheral wall portion of the flange mounting portion is diffusion bonded. A flange and a flange attaching part can be joined more firmly. Further, in the pressure vessel having a screw-in type sealing structure, the flange can be prevented from rotating.

In the pressure vessel inner cylinder according to the present invention, it is preferable that an adhesive layer made of platinum or a platinum alloy is further provided between the flange and the flange mounting portion. Diffusion bonding between the flange and the flange mounting portion can be performed more stably and efficiently in a shorter time.

In the inner cylinder for a pressure vessel according to the present invention, it is preferable that an adhesive layer made of platinum and an alloy of iridium, ruthenium, or iridium or ruthenium and platinum is provided between the flange and the flange mounting portion. . Diffusion bonding between the flange and the flange mounting portion can be performed more stably and efficiently in a shorter time.

The inner cylinder for a pressure vessel according to the present invention includes a form that is one or both of a lower inner cylinder provided in a main body of the pressure vessel and an upper inner cylinder provided in a lid of the pressure vessel.

The pressure vessel according to the present invention includes the inner tube for a pressure vessel according to the present invention.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present invention, the pressure vessel has a structure in which a sealed portion is formed by at least a bottomed cylindrical main body and a lid, and the inside of the pressure vessel is sealed. A covering portion that covers the inner surface, a flange mounting portion that extends in the centrifugal direction from the end portion of the covering portion, and an annular shape that is joined to the flange mounting portion and serves as a sealing portion of the seal portion A process for forming the covering portion and the flange mounting portion integrally with platinum or a platinum alloy, and the flange as iridium, ruthenium or iridium. Or the flange formation process formed with the alloy which consists of at least 1 sort (s) of ruthenium, and the cleaning process (cleaning proc) which cleans a joining plan surface among the surfaces of the said flange attaching part. ss), and the cleaned surface to be bonded and the surface of the flange are heated in a state in which the surface to be bonded is in contact with the metal element included in the flange mounting portion and included in the flange A bonding step of diffusing the metal element.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present invention, it is preferable to have a washing process for washing a planned joining surface among the surfaces of the flange before the joining step. Bonding can be performed more reliably.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present invention, it is preferable that the cleaning step includes a step of heat-treating a planned joining surface at 500 to 800 ° C. among the surfaces of the flange mounting portion. Impurities can be efficiently removed from the platinum surface.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present invention, the heat treatment in the cleaning step is preferably performed in an air atmosphere. Cleaning can be done without special equipment or equipment.

In the method for manufacturing a pressure vessel according to the present invention, before the joining step, further, a platinum compound or a platinum compound and a metal compound that forms an alloy with platinum are formed on the planned joining surface of the surface of the flange. A coating step of applying a coating solution to be dried and forming a coating layer; and a thermal decomposition step of thermally decomposing the coating layer to form an adhesion layer made of platinum or a platinum alloy to form a flange with an adhesion layer. It is preferable to have. Diffusion bonding between the flange and the flange mounting portion can be performed more stably and efficiently in a shorter time. Moreover, since the conditions of diffusion bonding can be eased, the flange attachment operation in a state where the covering portion and the flange attachment portion are attached to the pressure vessel is facilitated.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present invention, an iridium compound, a ruthenium compound, or an iridium is further formed on the planned joining surface among the surfaces of the flange mounting portion between the cleaning step and the joining step. A coating step in which a coating solution containing at least one compound or ruthenium compound and a platinum compound is coated and dried to form a coating layer; and the coating layer is thermally decomposed to at least one of iridium, ruthenium, iridium or ruthenium It is preferable to have a thermal decomposition step of forming an adhesion layer made of an alloy of seed and platinum and forming a flange mounting portion with an adhesion layer. Diffusion bonding between the flange and the flange mounting portion can be performed more stably and efficiently in a shorter time.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present invention, it is preferable that a diffusion step of heating at a temperature higher than the heating temperature of the pyrolysis step is further provided between the coating step and the joining step. Diffusion bonding can be performed more stably.

The present invention prevents the deformation of the flange, imparts durability, and can be used under supercritical conditions even if the material that covers the inner surface of the pressure vessel is different from the material that forms the flange. An inner cylinder for a pressure vessel that can withstand, and a method for manufacturing the same.

It is sectional drawing which shows an example of a large sized pressure vessel. (A) is the elements on larger scale of the seal | sticker part of the pressure vessel shown in FIG. 1, (b) is a top view which shows an example of the gasket used with the pressure vessel shown in FIG. It is a partial expanded sectional view which shows another form example of the junction part of the inner cylinder and flange of the pressure vessel shown in FIG. 1, (a) is an upper flange attachment part joined to the whole upper surface of an upper flange, The flange attachment part is a form that is joined to the entire bottom surface of the lower flange, and (b) is a form that the flange attachment part has a peripheral wall part, and the peripheral wall part and the outer peripheral surface of the flange are joined. It is sectional drawing which shows an example of a medium-sized pressure vessel. It is a partial expanded sectional view which shows the form example of the junction part of the inner cylinder of a pressure vessel shown in FIG. 4, and a flange, (a) is an upper flange attachment part joined to the whole upper surface of an upper flange, and lower flange attachment (B) is a form in which the flange mounting part has a peripheral wall part, and the peripheral wall part and the outer peripheral surface of the flange are joined. It is sectional drawing which shows an example of a small pressure vessel. It is a partial expanded sectional view which shows the form example of the junction part of the inner cylinder and flange of the pressure vessel shown in FIG. 6, (a) is the form which a flange attachment part joins to the whole surface of the top | upper surface or bottom face of a flange, (b ) Is a form in which the flange mounting portion has a peripheral wall portion, and the peripheral wall portion and the outer peripheral surface of the flange are joined.

Next, the present invention will be described in detail with reference to embodiments, but the present invention is not construed as being limited to these descriptions. As long as the effect of the present invention is exhibited, the embodiment may be variously modified.

FIG. 1 is a cross-sectional view showing an example of a large pressure vessel. The inner cylinder for a pressure vessel according to the present embodiment has a structure in which the pressure vessel 901 forms a seal portion with at least a bottomed cylindrical main body 81 and a lid 91 to seal the inside, and the pressure vessel 901 The cover portions 86 and 96 that cover the inner surface of the cover portion, the flange attachment portions 85 and 95 that extend in the centrifugal direction from the end portions of the cover portions 86 and 96, and the flange attachment portions 85 and 95; And the inner cylinder for pressure vessels provided with the annular flanges 84 and 94 used as the seal part of a seal part, and covering parts 86 and 96 and flange attaching parts 85 and 95 are processed integrally, and The flanges 84 and 94 are made of platinum or a platinum alloy, and the flanges 84 and 94 are made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium. A metal element contained in the di-mounting portion 85 and 95 is a diffusion bonding diffused.

The pressure vessel 901 is used as a vessel for chemical reaction such as synthesis, decomposition, and single crystal growth. The basic configuration of the pressure vessel 901 is as follows. The pressure vessel 901 has a main body 81 and a lid 91. The main body 81 has a bottomed cylindrical shape with an upper end opened. The lid 91 has a shape that can close the opening of the main body 81. The pressure vessel 901 has a structure in which the main body 81 and the lid 91 can be fixed with a fixing tool 72 such as a nut or a clamp to seal the inside. The main body 81 is heated by a heater (not shown) arranged on the outer periphery thereof. The main body 81, the lid 91, and the fixture 72 are generally made of a heat-resistant alloy such as low alloy steel or nickel chrome alloy.

An annular flange 84 (hereinafter referred to as a lower flange) is provided on the outer peripheral edge of the opening of the main body 81. In the pressure vessel 901 shown in FIG. 1, the lid 91 is provided with an annular flange 94 (hereinafter referred to as an upper flange) at a position corresponding to the lower flange 84. Fig.2 (a) is a partial expanded sectional view of the seal part of the pressure vessel shown in FIG. The lower flange 84 includes an outer peripheral surface 84a, an inner peripheral surface 84b, a top surface 84c connecting the upper end sides of the outer peripheral surface 84a and the inner peripheral surface 84b, and a bottom surface connecting the lower end sides of the outer peripheral surface 84a and the inner peripheral surface 84b. 84d. The top surface 84c has a top surface tapered portion 84c1. The bottom surface 84d has a bottom surface tapered portion 84d1. The upper flange 94 includes an outer peripheral surface 94a, an inner peripheral surface 94b, a top surface 94c connecting the upper end sides of the outer peripheral surface 94a and the inner peripheral surface 94b, and a bottom surface connecting the lower end sides of the outer peripheral surface 94a and the inner peripheral surface 94b. 94d. The top surface 94c has a top surface tapered portion 94c1. The bottom surface 94d has a bottom surface tapered portion 94d1. In addition, this invention is not restrict | limited to the shape of the upper flange 94 and the lower flange 84, unless the effect of this invention is impaired.

As shown in FIG. 2A, when the pressure vessel is sealed, the upper flange 94, the gasket 71a, and the lower flange 84 are in contact with each other by a line or a surface to form a seal portion (hereinafter referred to as a corresponding contact). The portion is referred to as a seal portion S). In FIG. 2A, the seal portion S is on the top taper portion 84 c 1 of the lower flange 84 and the bottom taper portion 94 d 1 of the upper flange 94. FIG. 2B is a plan view showing an example of a gasket used in the pressure vessel shown in FIG. In the pressure vessel 901, as shown in FIG. 2 (b), as the gasket 71a, the inner ring 77 and the inner ring 77 are made thinner than the inner ring portion on the outer peripheral side of the inner ring 77, which is called a graylock seal ring type. A self-tightening gasket having an outer ring 78 is used. The gasket 71a is generally made of a nickel-based alloy having heat and corrosion resistance. Since the gasket 71a has a portion that is directly exposed in the pressure vessel, at least the exposed surface is preferably a platinum group metal surface having corrosion resistance. Furthermore, the surface is more preferably a platinum group metal oxide. The present embodiment is not limited to the shape and material of the gasket 71a. However, in consideration of the durability of the inner cylinder, the gasket 71a preferably has a lower surface hardness than the upper flange 94 and the lower flange 84.

A pressure vessel 901 shown in FIG. 1 includes an inner cylinder 83 (hereinafter referred to as a lower inner cylinder) provided in a main body 81 and an inner cylinder 93 (hereinafter referred to as an upper inner cylinder) provided in a lid 91 as an inner cylinder for a pressure vessel. And). The covering portion 86 that covers the inner surface of the main body 81 is referred to as a lower covering portion. The lower covering portion 86 has a bottomed cylindrical shape with an upper end opened. The lower covering portion 86 is preferably formed along the inner wall of the main body 81. However, the shape of the bottom portion of the lower covering portion 86 is more preferably a hemispherical surface in terms of pressure resistance. Of the inner wall of the lid 91, the covering portion 96 that covers the area inside the inner peripheral surface 94b of the upper flange 94 is referred to as an upper covering portion. The upper covering portion 96 is preferably formed along the inner wall of the lid 91. In FIG. 1, the upper covering portion 96 has a planar circular shape. However, the present embodiment is not limited to the shape of the upper covering portion 96, and is, for example, hemispherical (dome shape) or cylindrical tube shape. be able to.

The flange mounting portion 85 extending in the centrifugal direction from the upper end portion of the lower coating portion 86 to the entire circumference is referred to as a lower flange mounting portion. The lower flange mounting portion 85 is processed into a shape that matches a part or all of the bottom surface 84d of the lower flange 84 to be joined or the bottom surface 84d and the outer peripheral surface 84a of the lower flange 84. The flange mounting portion 95 extending in the centrifugal direction from the end portion of the upper covering portion 96 to the entire circumference is referred to as an upper flange mounting portion. In FIG. 2A, the end portion of the upper covering portion 96 is a portion of the upper covering portion 96 that is in contact with the inner peripheral surface 94 b of the upper flange 94. The upper flange mounting portion 95 is processed into a shape that matches a part or all of the top surface 94c of the upper flange 94 to be joined or the top surface 94d and the outer peripheral surface 94a of the upper flange 94.

From here, the lower flange 84, the lower flange attaching part 85, and the lower coating | coated part 86 are demonstrated. As for the upper flange 94, the upper flange mounting portion 95, and the upper covering portion 96, the upper flange 94 is the lower flange 84, the upper flange mounting portion 95 is the lower flange mounting portion 85, and the upper covering portion 96 is the lower covering portion 86. Further, the same explanation can be made by replacing the bottom surface 84d of the lower flange 84 with the top surface 94c of the upper flange 94.

The lower covering portion 86 and the lower flange mounting portion 85 are integrally processed and have no joint portion. By integrally processing, the pressure resistance strength of the inner cylinder can be further increased. Furthermore, the lower coating | coated part 86 and the lower flange attaching part 85 are formed with platinum or a platinum alloy from the point of corrosion resistance, workability, and the fracture | rupture prevention at the time of use. Examples of the platinum alloy include a platinum-iridium alloy, a platinum-ruthenium alloy, a platinum-rhodium alloy, a platinum-gold alloy, and a platinum-rhenium alloy. The platinum alloy preferably has a platinum content in the alloy of 70% by mass or more. More preferably, it is 80 mass% or more. If it is less than 70 mass%, it may be inferior to corrosion resistance or workability.

The lower flange 84 is made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium having high pressure resistance and heat and corrosion resistance.

Alloys containing iridium (hereinafter referred to as iridium alloys) are, for example, iridium-ruthenium alloys, iridium-platinum alloys, iridium-rhodium alloys, iridium-gold alloys, iridium-rhenium alloys, iridium-platinum-rhodium alloys, iridium- Platinum-rhenium alloy, iridium-ruthenium-rhodium alloy, iridium-ruthenium-rhenium alloy, iridium-ruthenium-rhodium-platinum alloy. Ruthenium-containing alloys (hereinafter referred to as ruthenium alloys) are, for example, ruthenium-iridium alloys, ruthenium-platinum alloys, ruthenium-rhodium alloys, ruthenium-gold alloys, ruthenium-rhenium alloys, ruthenium-platinum-rhodium alloys, ruthenium- Platinum-rhenium alloy, ruthenium-iridium-rhodium alloy, ruthenium-iridium-rhenium alloy, ruthenium-iridium-rhodium-platinum alloy. The iridium alloy or ruthenium alloy preferably has an iridium content or ruthenium content in the alloy of 60% by mass or more. More preferably, it is 80 mass% or more. If it is less than 60 mass%, pressure resistance may be inferior.

In the inner cylinder for a pressure vessel according to the present embodiment, it is preferable that the surface of the seal portion S of the lower flange 84 has a Vickers hardness of 350 Hv or more measured according to JIS Z 2244: 2009. More preferably, it is 400 Hv or more. If it is less than 350 Hv, large deformation may occur due to tightening, and sufficient sealing may not be achieved. In addition, the surface hardness may be lower than that of the gasket 71a, and the flange may be deformed to shorten the life of the pressure vessel. The upper limit value of Vickers hardness is preferably 500 Hv. More preferably, it is 450 Hv.

The joining of the lower flange 84 and the lower flange attaching portion 85 is a diffusion joining in which a metal element contained in the lower flange 84 and a metal element contained in the lower flange attaching portion 85 are diffused. By diffusion bonding, the lower flange 84 and the lower flange mounting portion 85 are integrated, and the pressure resistance can be further increased. Further, as shown in FIG. 2 (a), the lower flange mounting portion 85 extends to a part of the bottom surface 84d of the lower flange 84, so that it is compared with butt welding as shown in FIG. As a result, the area of the joining portion increases, and a stronger joining becomes possible. Further, since no adhesive is used, there is no possibility that impurities will elute into the container. The joining area between the lower flange mounting portion 85 and the lower flange 84 is preferably 25% or more of the bottom surface 84d of the lower flange 84. More preferably, it is 30% or more. Particularly preferably, it is 50% or more. If it is less than 25%, the strength of the joint may be insufficient.

As shown in FIG. 2A, the lower flange mounting portion 85 may be bonded to a part of the bottom surface 84 d of the lower flange 84, but the lower flange mounting portion 85 is bonded to the entire bottom surface 84 d of the lower flange 84. More preferably. FIG. 3 is a partially enlarged cross-sectional view showing another embodiment of the joint portion between the inner cylinder and the flange of the pressure vessel shown in FIG. FIG. 3A shows a form in which the upper flange attaching portion 95 is joined to the entire top surface 94 c of the upper flange 94 and the lower flange attaching portion 85 is joined to the entire bottom surface 84 d of the lower flange 84. In the form shown in FIG. 3A, since the lower flange mounting portion 85 extends over the entire bottom surface 84d of the lower flange 84, the joining area is further increased and a stronger joining is possible. In addition, since the upper flange mounting portion 95 extends over the entire top surface 94c of the upper flange 94, the joining area is further increased, and a stronger joining is possible.

FIG. 3B shows a form in which the flange mounting portion has a peripheral wall portion, and the peripheral wall portion and the outer peripheral surface of the flange are joined. In the pressure vessel inner cylinder according to the present embodiment, the lower flange 84 has an outer peripheral surface 84a, the lower flange attachment portion 85 has a peripheral wall portion 85a processed integrally with the lower flange attachment portion 85, and The outer peripheral surface 84a of the lower flange 84 and the peripheral wall portion 85a of the lower flange mounting portion 85 are preferably diffusion bonded. Since the lower flange mounting portion 85 is joined over the entire bottom surface 84d of the lower flange 84 and the outer peripheral surface 84a of the lower flange 84, the joining can be made stronger.

In the inner tube for a pressure vessel according to the present embodiment, it is preferable to further provide an adhesion layer between the lower flange 84 and the lower flange mounting portion 85. The adhesion layer is preferably made of platinum or a platinum alloy, or made of iridium, ruthenium, or an alloy of platinum and at least one of iridium or ruthenium. By providing the adhesion layer, diffusion bonding between the lower flange 84 and the lower flange mounting portion 85 can be performed more stably and efficiently in a shorter time.

FIG. 4 is a cross-sectional view showing an example of a medium-sized pressure vessel. Since the basic structure of the medium-sized pressure vessel 902 shown in FIG. 4 is the same as that of the large-sized pressure vessel 901 shown in FIG. 1, the description of common points is omitted here, and different points will be described.

FIG. 5 is a partial enlarged cross-sectional view showing an example of a configuration of the joint portion between the inner cylinder and the flange of the pressure vessel shown in FIG. 4, and (a) shows that the upper flange mounting portion is joined to the entire top surface of the upper flange. The lower flange mounting portion is joined to the entire bottom surface of the lower flange, and (b) is a form in which the flange mounting portion has a peripheral wall portion and the peripheral wall portion and the outer peripheral surface of the flange are joined. In the pressure vessel 902 shown in FIGS. 4 and 5A and 5B, the lower flange 84 has a flat bottom surface 84d and has a bottom taper portion 84d1 of the pressure vessel 901 shown in FIGS. 1 and 2A. It is a form that does not. The upper flange 94 has a flat top surface 94c and does not have the top taper portion 94c1. In the pressure vessel 902, as the gasket 71b, a gasket called a lens ring having a thickest inner peripheral side of the ring and having a tapered section with a thickness decreasing toward the outer periphery is used. In the form shown in FIG. 5A, since the lower flange mounting portion 85 extends over the entire bottom surface 84d of the lower flange 84, the joining area is increased and strong joining is possible. In the form shown in FIG. 5B, the lower flange 84 has an outer peripheral surface 84a, the lower flange mounting portion 85 has a peripheral wall portion 85a processed integrally with the lower flange mounting portion 85, and Since the outer peripheral surface 84a of the flange 84 and the peripheral wall portion 85a of the lower flange mounting portion 85 are diffusion-bonded, the bonding area is further increased, and the lower flange 84 and the lower flange mounting portion 85 can be bonded more firmly. it can.

FIG. 6 is a cross-sectional view showing an example of a small pressure vessel. Since the basic structure of the small pressure vessel 903 shown in FIG. 6 is the same as that of the large pressure vessel 901 shown in FIG. 1, description of common points is omitted here, and different points will be described. The pressure vessel 903 shown in FIG. 6 is a form having only the lower inner cylinder 83 provided in the main body 81 of the pressure vessel 903 as an inner cylinder for a pressure vessel according to the present embodiment. The pressure vessel 903 is called a screw and bone type, and a gasket 71a as shown in FIGS. 1 to 3 or a gasket 71b as shown in FIGS. The projecting portion 99 provided on the lid 91 is fitted into the lower flange 84 without using the gasket, and is screwed and fixed to the screwing portion 88 provided on the outer periphery of the main body 81 with a fixing tool (cap nut) 73. And a structure for sealing the inside of the container. The convex part 99 has the surface of the oxide of a platinum group metal. The platinum group metal is preferably iridium, ruthenium, rhodium or a base alloy thereof. The oxides of the platinum group metals and their base alloys are, for example, iridium oxide, ruthenium oxide, rhodium oxide, iridium oxide / platinum, iridium ruthenium oxide, iridium rhodium oxide, iridium rhenium oxide, iridium oxide / gold.

The pressure vessel 903 is sealed by coming into contact with the projecting portion 99 and the lower flange 84 via a bonding prevention material 89 at a seal location S. The anti-bonding member 89 has a role of preventing the convex portion 99 and the lower flange 84 from being bonded during use of the pressure vessel. Further, as described above, the lower flange 84 is made of metal, and the surface of the convex portion 99 is an oxide. Therefore, in principle, the lower flange 84 and the convex portion 99 are not bonded, but in order to further prevent joining. Further, a corrosion-resistant nitride such as BN or TaN can be interposed.

FIG. 7 is a partially enlarged cross-sectional view showing an example of a configuration of a joint portion between the inner cylinder and the flange of the small pressure vessel shown in FIG. 6, and (a) shows the flange mounting portion on the entire top surface or bottom surface of the flange. In the form to be joined, (b) is a form in which the flange mounting part has a peripheral wall part and the peripheral wall part and the outer peripheral surface of the flange are joined. In the pressure vessel 903 shown in FIGS. 6 and 7A and 7B, the bottom flange 84 has a flat bottom surface 84d and has a bottom taper portion 84d1 of the pressure vessel 901 shown in FIGS. 1 and 2A. It is a form that does not. In the form shown in FIG. 7A, since the lower flange mounting portion 85 extends to the bottom surface 84d of the lower flange 84, the joining area is increased and strong joining is possible. FIG. 7A shows a form in which the lower flange attachment portion 85 is joined to the entire bottom surface 84d of the lower flange 84. However, the present embodiment is not limited to this, and the lower flange attachment portion 85 has the lower flange 84. What is necessary is just to join to a part of 84 d of bottom surfaces.

In the form shown in FIG. 7B, the lower flange 84 has an outer peripheral surface 84a, the lower flange mounting portion 85 has a peripheral wall portion 85a processed integrally with the lower flange mounting portion 85, and Since the outer peripheral surface 84a of the flange 84 and the peripheral wall portion 85a of the lower flange mounting portion 85 are diffusion-bonded, the bonding area is further increased, and the lower flange 84 and the lower flange mounting portion 85 can be bonded more firmly. it can. Furthermore, the lower flange 84 can be prevented from rotating by screwing and fixing the fixture (cap nut) 73.

The pressure vessel according to the present embodiment includes the inner tube for the pressure vessel according to the present embodiment. The inner cylinder for a pressure vessel according to the present embodiment covers the inner surface with platinum or a platinum alloy having excellent corrosion resistance and extensibility, so that it is easy to process and occurs between the main body and the coating portion due to a temperature rise. Damage to the inner cylinder due to the expansion difference can be prevented. Since the flange is formed of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium having high physical strength and excellent chemical stability, the deformation of the flange is small even when used repeatedly. Since the flange mounting part and the flange processed integrally with the cover part are integrated by diffusion bonding, it can withstand use under ultra-high temperature and ultra-high pressure conditions. Therefore, in the pressure vessel according to the present embodiment, the frequency of readjustment and maintenance of the seal portion is low, the inner cylinder has a long life, and the time and labor devoted to maintenance can be reduced.

Next, a method for manufacturing a pressure vessel inner cylinder according to the present embodiment will be described. The method for manufacturing an inner cylinder for a pressure vessel according to the present embodiment has a structure in which the pressure vessel forms a seal portion with at least a bottomed cylindrical main body and a lid to seal the inside, and the pressure vessel A cover portion covering the inner surface of the cover portion, a flange mounting portion extending in the centrifugal direction over the entire circumference from the end portion of the cover portion, and joining to the flange mounting portion and serving as a sealing portion of the seal portion A pressure vessel inner cylinder comprising: an annular flange, wherein the covering portion and the flange mounting portion are integrally formed of platinum or a platinum alloy; and the flange is iridium, ruthenium or A flange forming step formed of an alloy made of at least one of iridium or ruthenium, a cleaning step of cleaning a planned joining surface among the surfaces of the flange mounting portion, and the cleaned bonding preparatory step. A joining step of heating the surface of the flange and the surface of the flange in contact with the surface to be joined and diffusing the metal element contained in the flange mounting portion and the metal element contained in the flange; Have. Here, the inner cylinder is, for example, the lower inner cylinder 83 of the pressure vessels 901, 902, and 903 shown in FIGS. 1, 4, and 6, and the upper inner cylinder of the pressure vessels 901 and 902 shown in FIGS. 93.

The processing step is a step in which the covering portion and the flange mounting portion are integrally processed without forming a joint portion with platinum or a platinum-based alloy. A processing method is not specifically limited, For example, it is a generally well-known metal processing method, such as a casting method, a forging method, and a press molding method. The thicknesses of the covering portion and the flange mounting portion are not particularly limited, and are, for example, 0.2 to 10 mm. As for the thickness of a coating | coated part and a flange attaching part, the whole may be uniform and thickness may be changed partially. When the thickness is partially changed, for example, the flange mounting portion can be reinforced to be thicker than the covering portion. At this time, the thickness of the thinnest portion (for example, the side wall portion of the covering portion) is preferably 0.2 to 5 mm.

In the flange forming step, the flange is formed of iridium, ruthenium, or an alloy made of at least one of iridium or ruthenium. A processing method is not specifically limited, For example, it can form with the above-mentioned general well-known metal processing method. The shape and dimensions of the flange are designed according to the shape of the pressure vessel to be installed, the maximum operating pressure and the capacity, and are not particularly limited as long as the shape and size can form a seal portion when sealing the opening of the pressure vessel. .

The cleaning step is a step of cleaning the surface to be joined with the flange among the surfaces of the flange mounting portion. By cleaning, the metal contained in the flange mounting portion and the metal contained in the flange are likely to diffuse. When the surface of platinum or a platinum alloy is heated at 500 ° C. or higher, the surface oxide is removed. Therefore, it is preferable to utilize this property for cleaning in that impurities can be efficiently removed from the platinum surface. That is, in the method for manufacturing a pressure vessel inner cylinder according to the present embodiment, the cleaning step preferably includes a step of heat-treating a planned joining surface at 500 to 800 ° C. of the surface of the flange mounting portion. Note that the heat treatment in the cleaning step can be performed in an atmosphere from which oxygen is removed or in an air atmosphere, but the cleaning can be performed efficiently without the need for special equipment or equipment. It is more preferable to carry out in an air atmosphere. Even in an air atmosphere containing oxygen, platinum or a platinum alloy has the above-described characteristics, so that the metal surface can be exposed without forming an oxide.

The joining process is a process in which the cleaned flange mounting part and the cleaned flange are completely overlapped and heated so that there is no gap, and the metal element contained in the flange mounting part and the metal element contained in the flange are diffused. is there. The joining conditions are not particularly limited. For example, heating is performed at 900 to 1500 ° C. while pressurizing at 10 ⁶ to 10 ⁷ Pa. The pressurization method may be any method that allows uniform pressurization, for example, a method using hot isostatic pressing (HIP), a hot press method, or a vise. In addition, it is preferable to perform a joining process in nitrogen or argon atmosphere.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present embodiment, it is preferable to have a cleaning step of cleaning the surfaces to be bonded out of the flange surfaces before the bonding step. By washing, it is possible to prevent bonding failure caused by surface deposits. The cleaning method is not particularly limited, and examples thereof include a method using a cleaning agent, a method using a solvent, a method using a chemical reaction, and a mechanical method such as polishing.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present embodiment, before the joining step, (1) a platinum compound or (2) a platinum compound and an alloy of platinum and alloy on the planned joining surface of the flange surface. An application step (hereinafter referred to as application step A) of applying a coating solution containing a metal compound that forms a coating and drying to form an application layer, and an adhesion made of platinum or a platinum alloy by thermally decomposing the application layer It is preferable to have a layer (hereinafter referred to as adhesion layer A) and a thermal decomposition step (hereinafter referred to as thermal decomposition step A) for forming a flange with the adhesion layer A. Diffusion bonding between the flange and the flange mounting portion can be performed more stably and efficiently in a shorter time. Moreover, since the conditions of diffusion bonding can be eased, the flange attachment operation in a state where the covering portion and the flange attachment portion are attached to the pressure vessel is facilitated. For example, in the form in which the adhesion layer A is not provided, the heating temperature for diffusion bonding is 900 to 1500 ° C., but in the form in which the adhesion layer A is provided, the heating temperature can be 600 ° C. or more and less than 900 ° C.

In the coating step A, a coating solution containing a platinum compound or a coating solution containing a platinum compound and a metal compound that forms an alloy with platinum is applied on the surface to be bonded, and dried. And forming a coating layer. The coating step A is preferably performed after the cleaning step without passing through other steps. The method for applying the coating solution is a generally known method such as dipping, coating, or spraying. The drying method is a generally known method such as a natural drying method, a heat drying method, or a vacuum drying method. In the case of heat drying, it is preferable to heat at a temperature lower than the heating temperature in the thermal decomposition step A to be performed later. In the present embodiment, the application method and the drying method are not limited.

The platinum compound is, for example, chloroplatinic acid or dinitrodiammine platinum. Examples of the metal compound that forms an alloy with platinum include an iridium compound, a ruthenium compound, a rhodium compound, a gold compound, and a rhenium compound. Examples of the iridium compound include iridium chloride, iridium nitrate, chloroiridic acid, iridium butoxide, and the like. Examples of the ruthenium compound include ruthenium chloride, ruthenium nitrate, ruthenium chloride, ruthenium butoxide, and the like. The rhodium compound is, for example, rhodium chloride or rhodium nitrate. Examples of the gold compound include chloroauric acid, gold chloride, and gold cyanide. The rhenium compound is, for example, rhenium chloride or rhenium nitrate. A solvent is not specifically limited, For example, they are water, nitric acid water, hydrochloric acid water, alcohol, turpentine oil, or those liquid mixture. When a solution containing only a platinum compound is used as the coating solution, the obtained adhesion layer A is a layer made of platinum. When a solution containing a platinum compound and a metal compound that forms an alloy with platinum is used as the coating solution, the resulting adhesive layer A is a layer made of a platinum alloy. The type of compound contained in the coating solution is not particularly limited in the present embodiment as long as the adhesion layer A made of platinum or a platinum alloy can be formed by thermal decomposition performed later.

In the thermal decomposition step A, the coating layer is made into an adhesion layer A made of platinum or a platinum alloy by thermal decomposition. Pyrolysis can be performed in a heating furnace such as a muffle furnace. The heating temperature is preferably 300 to 800 ° C. More preferably, it is 500 to 700 ° C. The treatment time varies depending on the temperature and the components of the coating solution, but is preferably 5 to 15 minutes. It does not matter whether the thermal decomposition is in an air atmosphere or a reducing atmosphere.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present embodiment, a diffusion step (hereinafter referred to as “heating” the flange with the adhesion layer A at a temperature higher than the heating temperature in the pyrolysis step between the coating step and the joining step). And a diffusion step A). In the diffusion step A, the flange with the adhesion layer A is heated at a temperature higher than the heating temperature in the pyrolysis step to diffuse the metal element contained in the flange and the metal element contained in the adhesion layer A. Integrate with the flange. The heating temperature in the diffusion step is preferably 650 to 900 ° C. More preferably, it is 700 to 800 ° C. The treatment time varies depending on the temperature and the components of the adhesion layer A, but is preferably 1 to 5 hours. When the heating temperature is less than 650 ° C., diffusion does not occur, the interlayer strength between the adhesion layer A and the flange is insufficient, and peeling may occur when used under high temperature and high pressure conditions. If it exceeds 900 ° C., a lot of energy is required for heating, which is uneconomical in balance with the degree of diffusion. Moreover, it does not ask | require whether the atmosphere of a spreading | diffusion process is in an air atmosphere or a reducing atmosphere.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present embodiment, an iridium compound, a ruthenium compound, an iridium compound or Applying a coating solution containing at least one ruthenium compound and a platinum compound and drying to form a coating layer (hereinafter referred to as coating step B); and thermally decomposing the coating layer, iridium, ruthenium or A thermal decomposition step (hereinafter referred to as a thermal decomposition step B) for forming a flange mounting portion with the adhesive layer B as an adhesive layer (hereinafter referred to as an adhesive layer B) made of an alloy of at least one of iridium or ruthenium and platinum. It is preferable to have.

The coating process B includes a coating solution containing an iridium compound, a coating solution containing a ruthenium compound, a coating solution containing an iridium compound and a platinum compound, a coating solution containing a ruthenium compound and a platinum compound, or an iridium compound, a ruthenium compound and platinum. In this process, the coating solution containing the compound is applied onto the surface to be bonded in the cleaned surface of the flange mounting portion and dried to form a coating layer. It is preferable to perform the application process B without passing through other processes after the cleaning process. The method of applying the coating liquid and the method of drying are the same as in the coating step A.

The type of iridium compound, ruthenium compound, platinum compound and solvent to be contained in the coating solution is not limited as long as the adhesion layer B made of an alloy of iridium, ruthenium, iridium or ruthenium and platinum can be formed by thermal decomposition performed later. The compound and the solvent exemplified in the coating step A can be appropriately selected.

In the thermal decomposition step B, the coating layer is made into an adhesion layer B made of platinum and an alloy of iridium, ruthenium, iridium or ruthenium and platinum. Pyrolysis conditions are the same as in pyrolysis step A.

In the method for manufacturing an inner cylinder for a pressure vessel according to the present embodiment, a diffusion step of heating the flange mounting portion with the adhesion layer B at a temperature higher than the heating temperature of the pyrolysis step between the coating step and the joining step. (Hereinafter referred to as diffusion step B) is preferable. In the diffusion step B, the metal element contained in the flange mounting portion and the metal element contained in the adhesion layer B are diffused to integrate the adhesion layer B and the flange. The diffusion conditions are the same as in the diffusion step A.

The coating process A, the thermal decomposition process A, the coating process B, and the thermal decomposition process B may be performed independently or both. Specifically, in the application process A and the thermal decomposition process A, the adhesion layer A is formed on the planned joining surface of the flange, and the adhesion layer A and the planned joining surface of the flange mounting portion are brought into contact with each other, and the application process In the coating process A and the thermal decomposition process A, the adhesion layer B is formed on the planned joining surface of the flange mounting portion in B and the thermal decomposition process B, and the planned joining surface of the flange and the adhesion layer B are brought into contact with each other. The adhesion layer A is formed on the flange bonding planned surface, and the adhesion layer B is formed on the bonding bonding surface of the flange mounting portion in the coating process B and the thermal decomposition process B, and the adhesion layer A and the adhesion layer B are brought into contact with each other Are joined together.

The thickness of the adhesion layer (adhesion layer A or adhesion layer B) is preferably 0.5 to 10 μm. More preferably, it is 1 to 3 μm. It is preferable to repeat the coating process and the thermal decomposition process a plurality of times until the thickness is reached. A uniform adhesion layer with few pores can be obtained. If it is less than 0.5 μm, the effect of providing an adhesion layer may not be obtained. If it exceeds 10 μm, durability may be reduced due to cohesive failure of the adhesion layer. Also, the pores of the adhesion layer may increase and the diffusion effect may decrease. In addition, the strength of the adhesion layer portion may be insufficient.

Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not construed as being limited to the examples.

Example 1
The covering portion and the flange mounting portion were integrally processed with a thickness of 0.2 mm using platinum so as to follow the inner wall of the autoclave main body used at high temperature and high pressure. In addition, in the Example, the autoclave used the small pressure vessel shown in FIG. 6 in common. On the other hand, the flange was formed with a thickness of 5.0 mm using iridium. The Vickers hardness at the flange seal portion was 410 Hv. The surface to be joined of the flange mounting part is washed with a neutral detergent (trade name EMAL, manufactured by Kao Corporation) and heated in air at 600 ° C to remove surface deposits and surface oxides. And cleaned. The surface to be joined of the flange was polished and cleaned. In a state where the cleaned planned joining surface of the flange mounting portion and the cleaned planned joining surface of the flange are in contact with each other, they are assembled as shown in FIG. 6 and tightened and fixed to a pressure of 10 ⁷ Pa. In the heating furnace, the joining process was performed for 2 hours at 900 degreeC in the air | atmosphere. After the treatment, it was allowed to cool with pressure applied. In the obtained inner cylinder, the platinum flange mounting portion and the iridium flange were completely fixed and integrated.

(Example 2)
A covering portion, a flange mounting portion, and a flange were prepared in the same manner as in Example 1. The surface to be joined of the flange mounting part is washed with a neutral detergent (trade name EMAL, manufactured by Kao Corporation) and heated in air at 600 ° C to remove surface deposits and surface oxides. And cleaned. The surface to be joined of the flange is washed with a neutral detergent (trade name Emar, manufactured by Kao Corporation) in the same manner as described above. did. Subsequently, thermal decomposition was performed by heating at 700 ° C. for 30 minutes in a muffle furnace in which air was passed. The coating-pyrolysis was repeated three times to form an adhesion layer made of platinum having a thickness of 0.2 μm on the surface of the iridium flange. Furthermore, it heated at 900 degreeC for 2 hours, the diffusion process was performed, the iridium of a flange, and platinum of an adhesion layer were diffused, and the flange with an adhesion layer was obtained. In the state which contact | adhered the joining plan surface of the cleaned flange mounting part, and the contact | adherence layer of the flange with an adhesion | attachment layer, it fixed with the fixture which kept the pressure using the spring washer. In the flame reduction furnace, the joining process was performed at a heating temperature of 600 ° C. and a pressure of 9.8 × 10 ⁶ Pa for 2 hours. After the treatment, it was allowed to cool with pressure applied. In the obtained inner cylinder, the platinum flange mounting portion and the iridium flange were completely fixed and integrated. Moreover, since the adhesion layer was provided, the heating temperature of the bonding process could be lowered as compared with Example 1 in which the adhesion layer was not provided.

(Example 3)
The covering portion and the flange mounting portion were integrally processed with a thickness of 0.2 mm using an alloy of 80% by mass of platinum and 20% by mass of gold so as to follow the inner wall of the autoclave used at high temperature and high pressure. On the other hand, the flange was formed with a thickness of 2.0 mm using an alloy of 80% by mass of iridium and 20% by mass of platinum. The Vickers hardness of the flange seal portion was 450 Hv. The surface to be joined of the flange mounting portion was washed with acetone (special grade reagent manufactured by Wako Pure Chemical Industries, Ltd.) and then heated in air at 600 ° C. to remove surface deposits and to remove surface oxides for cleaning. . In the same manner as in Example 1, an adhesion layer made of platinum was formed on the surface to be joined of the flange, and a diffusion-treated flange was obtained without performing diffusion treatment. The pressure was fixed in the same manner as in Example 2 in a state where the cleaned planned joining surface of the flange mounting portion and the adhesion layer of the flange with the adhesion layer were in contact with each other. Joining treatment was performed for 3 hours at a heating temperature of 900 ° C. and a pressure of 9.8 × 10 ⁶ Pa in a reducing furnace in which a reducing gas obtained by adding 10 atomic% of hydrogen to argon gas was circulated. After the treatment, it was allowed to cool with pressure applied. In the obtained inner cylinder, the platinum-gold alloy flange mounting portion and the iridium-platinum alloy flange were completely fixed and integrated.

Example 4
The covering portion and the flange mounting portion were integrally processed with a thickness of 0.2 mm using platinum so as to follow the inner wall of the autoclave used at high temperature and high pressure. On the other hand, the flange was formed with a thickness of 5.0 mm using an alloy of 80% by mass of ruthenium and 20% by mass of platinum. The Vickers hardness of the sealing part of the flange was 490 Hv. The surface to be joined of the flange is washed with acetone (special grade reagent manufactured by Wako Pure Chemical Industries), and the dinitrodiammine platinum is dissolved in water and n-propyl alcohol so that the platinum on the surface to be joined becomes 100 g / l. The liquid was applied and dried at 60 ° C. Subsequently, thermal decomposition was performed by heating at 400 ° C. for 15 minutes in a muffle furnace in which air was passed. The coating-pyrolysis was repeated three times to form an adhesion layer made of platinum having a thickness of 0.2 μm on the surface of the ruthenium-platinum alloy flange. Furthermore, it heated at 800 degreeC in argon gas atmosphere for 2 hours, the diffusion process was performed, the ruthenium-platinum alloy of a flange and platinum of an adhesion layer were diffused, and the flange with an adhesion layer was obtained. It fixed to the self-made press apparatus in the state which contact | abutted the joining plan surface of the cleaned flange mounting part, and the contact | adherence layer of the flange with the contact | adherence layer. The pressure was set to 10 ⁶ to 10 ⁷ Pa. A flame having a temperature of about 800 ° C. was sent to the joined portion and heated and joined for 2 hours. Note that the temperature at the joint was slightly maintained, but was generally maintained at 770 to 830 ° C. After the treatment, it was allowed to cool with pressure applied. In the obtained inner cylinder, the platinum flange mounting portion and the ruthenium-platinum alloy flange were completely fixed and integrated.

In Examples 1 to 4, the small pressure vessel inner cylinder shown in FIG. 6 was produced. However, the pressure vessel inner cylinder installed on the main body and lid of the large pressure vessel shown in FIG. A pressure vessel inner cylinder installed on the main body and lid of the pressure vessel could be produced in the same manner.

In the pressure vessel inner cylinder according to the present invention, the flange is formed of iridium having a high surface hardness, ruthenium, or an alloy containing at least one iridium or ruthenium, preventing deformation of the flange, and imparting durability. The material that coats the inner surface of the pressure vessel is made of platinum or platinum alloy with excellent workability and extensibility to prevent breakage during use, and the flange mounting part and the flange are integrated by diffusion bonding. Suitable as an inner cylinder for pressure vessels used under critical conditions.

71a gasket 71b gasket 72 fixture 73 fixture (cap nut)
77 Inner ring 78 Outer ring 81 Main body 83 Lower inner cylinder 91 Lid 84 Lower flange 84a Lower flange outer peripheral surface 84b Lower flange inner peripheral surface 84c Lower flange top surface 84c1 Lower flange top taper portion 84d Lower flange bottom surface 84d1 Lower flange Bottom flange mounting portion 85a lower flange mounting portion 85a peripheral wall portion 86 of lower flange mounting portion lower covering portion 88 screwing portion 89 joint preventing material 93 upper inner cylinder 94 upper flange 94a upper flange outer peripheral surface 94b upper flange inner peripheral surface 94c Upper flange top surface 94c1 Upper flange top taper portion 94d Upper flange bottom surface 94d1 Upper flange bottom taper portion 96 Upper covering portion 95 Upper flange mounting portion 99 Convex portion 901 Pressure vessel 902 Pressure vessel 903 Pressure vessel S Seal location

Claims (14)

The pressure vessel has a structure that forms a seal portion with at least a bottomed cylindrical main body and a lid to seal the inside, and a covering portion that covers the inner surface of the pressure vessel, and an end of the covering portion An inner cylinder for a pressure vessel comprising: a flange mounting portion extending in a centrifugal direction over the entire circumference; and an annular flange which is joined to the flange mounting portion and serves as a seal portion of the seal portion. ,
The covering portion and the flange mounting portion are integrally processed, and are made of platinum or a platinum alloy,
The flange is made of iridium, ruthenium, or an alloy containing at least one of iridium or ruthenium,
The inner tube for a pressure vessel, wherein the joining is diffusion joining in which a metal element contained in the flange and a metal element contained in the flange mounting portion are diffused. 2. The inner cylinder for a pressure vessel according to claim 1, wherein the surface of the seal portion of the flange has a Vickers hardness of 350 Hv or more measured according to JIS Z 2244: 2009. The flange has an outer peripheral surface, the flange mounting portion has a peripheral wall portion processed integrally with the flange mounting portion, and the outer peripheral surface of the flange and the peripheral wall portion of the flange mounting portion are diffused. The pressure cylinder inner cylinder according to claim 1 or 2, wherein the inner cylinder is joined. The pressure vessel inner cylinder according to any one of claims 1 to 3, further comprising an adhesion layer made of platinum or a platinum alloy between the flange and the flange mounting portion. The adhesive layer according to any one of claims 1 to 4, further comprising an adhesion layer made of an alloy of iridium, ruthenium, or at least one of iridium or ruthenium and platinum between the flange and the flange mounting portion. An inner cylinder for a pressure vessel as described in 1. 6. The pressure vessel inner cylinder according to any one of claims 1 to 5, wherein both or any of a lower inner cylinder provided in a main body of the pressure vessel and an upper inner cylinder provided in a lid of the pressure vessel. An inner cylinder for a pressure vessel, which is one of them. A pressure vessel comprising the pressure vessel inner cylinder according to any one of claims 1 to 6. The pressure vessel has a structure that forms a seal portion with at least a bottomed cylindrical main body and a lid to seal the inside, and a covering portion that covers the inner surface of the pressure vessel, and an end of the covering portion Manufacturing method of an inner cylinder for a pressure vessel, comprising: a flange mounting portion extending in a centrifugal direction from the portion to the centrifugal direction; and an annular flange joined to the flange mounting portion and serving as a sealing portion of the seal portion Because
A processing step of integrally forming the covering portion and the flange mounting portion with platinum or a platinum alloy,
Forming the flange with iridium, ruthenium, or an alloy of at least one of iridium or ruthenium; and
Of the surface of the flange mounting portion, a cleaning process for cleaning the planned joining surface,
Heating the cleaned planned joining surface and the flange surface out of contact with the joining planned surface, the metal element contained in the flange mounting portion and the metal element contained in the flange A diffusion process to diffuse;
A method for manufacturing an inner cylinder for a pressure vessel, comprising: The method for manufacturing an inner cylinder for a pressure vessel according to claim 8, further comprising a cleaning step of cleaning a surface to be bonded out of the surfaces of the flange before the bonding step. The production of an inner cylinder for a pressure vessel according to claim 8 or 9, wherein the cleaning step includes a step of heat-treating a bonding scheduled surface among the surfaces of the flange mounting portion at 500 to 800 ° C. Method. The method for manufacturing an inner cylinder for a pressure vessel according to claim 10, wherein the heat treatment in the cleaning step is performed in an air atmosphere. Before the joining step,
Applying a coating liquid containing a platinum compound or a platinum compound and a metal compound that forms an alloy with platinum on the surface to be joined among the surfaces of the flange, and drying to form a coating layer;
A thermal decomposition step of thermally decomposing the coating layer to form an adhesive layer made of platinum or a platinum alloy, and forming a flange with an adhesive layer;
The method for producing an inner cylinder for a pressure vessel according to any one of claims 8 to 11, wherein: Between the cleaning step and the joining step,
The application | coating liquid which apply | coats the coating liquid containing at least 1 sort (s) of an iridium compound, a ruthenium compound, or an iridium compound or a ruthenium compound, and a platinum compound on the joining plan surface among the surfaces of the said flange attachment part, and drys and forms a coating layer Process,
A thermal decomposition step of thermally decomposing the coating layer to form an adhesive layer comprising an alloy of iridium, ruthenium, or at least one of iridium or ruthenium and platinum, and forming a flange mounting portion with the adhesive layer;
The method for producing an inner cylinder for a pressure vessel according to any one of claims 8 to 12, wherein: Between the application step and the joining step,
The method for producing an inner cylinder for a pressure vessel according to claim 12 or 13, further comprising a diffusion step of heating at a temperature higher than the heating temperature of the pyrolysis step.

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