JP2019081683A - Method for producing high-temperature seal member, and high-temperature seal member - Google Patents

Abstract

To provide a seal member for gas seal, used for a high-temperature part, especially to provide: a method for producing a high-temperature seal member excellent in thermal insulating properties and capable of ensuring sufficient sealability, as a seal member comprising a ceramic-based composite material; and the high-temperature seal member.SOLUTION: A method for producing a high-temperature seal member 10B includes: an impregnation step of impregnating a liquid matter, which comprises an oxide ceramic powder or an oxide ceramic product, in a fiber aggregate, which is formed by entwining non-oxide inorganic fibers irregularly, to form an impregnated body; and a baking step of baking the impregnated body. Preferably, the method for producing the high-temperature seal member 10B includes: arranging the impregnated body at a position where the seal member 10B to be the product in an actual machine should be installed, in a step prior to the baking step; and then baking the impregnated body through a heat to be added to the impregnated body during the operation of the actual machine as the baking step.SELECTED DRAWING: Figure 3

Description

  The present invention relates to a method of manufacturing a high temperature seal member for gas sealing, and a high temperature seal member in an apparatus operated or used at high temperature such as a gas turbine.

  In a gas turbine, in order to increase its efficiency, sealing members for performing gas sealing, such as gaskets and seal plates, are used at various places. Heretofore, as this type of seal member is generally exposed to high temperatures, it has been common to use a metal having heat resistance, such as various heat resistant steels or Ni-based superalloys.

On the other hand, in recent years, attempts have been made to use ceramic matrix composites (CMCs) with excellent heat insulation and heat resistance for parts of high temperature parts in gas turbines, such as split rings and heat shield rings of stator blades.
As a method of manufacturing a member made of a ceramic matrix composite, there is a method in which a sheet made of ceramic fibers as a fiber reinforcing material is impregnated with a slurry of ceramic powder, pressed if necessary, formed, heated and fired. It is common. Moreover, it is common to arrange and use the member which consists of such a ceramic base composite material in the high temperature site | part of real machines, such as a gas turbine, in the state finished to the form of the product after the baking. And as a sheet which consists of a ceramic fiber used for the above manufacturing methods, as patent document 1 shows, it is common to use the woven fabric which woven the long fiber of the ceramic fiber as a warp and a weft. is there.

JP 2002-234777 A

  By the way, the present inventors have attempted to use a ceramic matrix composite material in place of metal as a seal member at a high temperature portion of a gas turbine. Ceramic-based composite materials have lower thermal conductivity and superior thermal insulation compared to metals, so if they are used as sealing members in high-temperature areas, they can exhibit thermal insulation as well as gas sealing. it is conceivable that.

  However, it has been recognized that when a ceramic matrix composite material is used in place of metal as a seal member at a high temperature portion of a gas turbine, a problem in terms of sealability actually occurs. That is, it has been found that when the conventional general ceramic base composite material is used for the seal member, a gap is easily generated between the surface of the seal member and the mating material, and the sealability can not be sufficiently secured. Therefore, in the conventional general ceramic base composite material, although being excellent in heat insulation much more than metal, it has been deterred to use as a sealing member of a gas turbine.

  The present invention has been made against the background described above, and as a sealing member for gas sealing used in high temperature parts, particularly as a sealing member made of a ceramic matrix composite material, it is excellent in heat insulation and sufficiently sealing performance. It is an object of the present invention to provide a method for manufacturing a high temperature seal member capable of securing the high temperature seal member and a high temperature seal member.

In order to solve the above problems, the inventors of the present invention have conducted intensive experiments and studies, and as a fiber assembly for fiber reinforcement, not a woven fabric but a fiber assembly in which short fibers are randomly intertwined, that is, generally Using non-woven fabric or fiber assembly called felt, and using non-oxide inorganic fiber represented by SiC (silicon carbide) as the fiber, and oxide ceramic as composite material matrix ceramic By using, it discovered that the said subject could be solved, and came to form one aspect of invention.
Furthermore, it has been found that sealing performance can be further improved by making the step of performing the firing step of the manufacturing process different from the step of the firing step in the conventional general method, and another aspect of the present invention. I came to

Specifically, the method for manufacturing the high temperature sealing member of the basic aspect (first aspect) of the present invention is
An impregnation step of impregnating a fiber assembly comprising non-oxide inorganic fibers randomly intertwined with an oxide-based ceramic powder or a liquid containing an oxide-based ceramic material to form an impregnated body; And a firing step of firing the sheet.

  In the method for producing a high temperature sealing member according to the second aspect of the present invention, in the method for producing a high temperature sealing member according to the first aspect, the non-oxide inorganic fiber is a SiC-based fiber. Do.

  Further, in the method for producing a high temperature seal member according to the third aspect of the present invention, in the method for producing a high temperature seal member according to the first or second aspect, the oxide material ceramic is used as the liquid in the impregnating step. It is characterized by using a slurry in which the powder is suspended in a dispersion medium.

  In the method for manufacturing a high temperature sealing member according to the fourth aspect of the present invention, in the method for manufacturing a high temperature sealing member according to the first or second aspect, an oxide-based material is used as the liquid in the impregnating step. It is characterized by using a ceramic precursor solution or a metal salt solution for producing an oxide-based ceramic.

  In the method for manufacturing a high temperature sealing member according to the fifth aspect of the present invention, in the method for manufacturing a high temperature sealing member according to any one of the first to fourth aspects, the impregnated body is A seal member in an actual machine is disposed at a place to be mounted, and the impregnated body is sintered by the heat applied to the impregnated body during the operation of the actual machine as the firing step.

  In the method for manufacturing a high temperature seal member according to the sixth aspect of the present invention, in the method for manufacturing a high temperature seal member according to any one of the first to fourth aspects, the method is used prior to mounting on a real machine as a high temperature seal member for products. The above-mentioned firing step is carried out at the stage of

  In the method for manufacturing a high temperature seal member according to a seventh aspect of the present invention, in the method for manufacturing a high temperature seal member according to any one of the first to sixth aspects, the high temperature seal member is used for a gas turbine It is characterized by being a member.

  Further, in the high temperature sealing member according to the eighth aspect of the present invention, in the fiber aggregate consisting of irregularly intertwined non-oxide inorganic fibers, the void portion between the fibers is filled with oxide ceramic, And the ceramic are sinter-bonded.

  According to the method for producing a high temperature sealing member of one aspect of the present invention, as a sealing member made of a ceramic matrix composite material for gas sealing used for high temperature parts, it has excellent heat insulation and sufficient sealing performance. It is possible to obtain a high temperature sealing member capable of securing the

It is a perspective view which shows a gasket as an example of the sealing member for high temperatures manufactured by the manufacturing method of 1st embodiment of this invention. It is a general | schematic longitudinal cross-sectional view which shows the use aspect of the gasket of FIG. It is a schematic diagram which shows the whole process of the manufacturing method of the high temperature sealing member of 1st embodiment of this invention. It is a general | schematic longitudinal cross-sectional view which shows the use aspect of the seal plate as an example of the sealing member for high temperatures manufactured by the manufacturing method of 2nd embodiment of this invention.

First Embodiment
First, the first embodiment will be described with reference to FIGS. 1 to 3.
The high temperature sealing member manufactured by the manufacturing method of the present invention is a sealing member disposed for gas sealing at a high temperature portion of a gas turbine or the like, and, for example, a gasket, a split ring on the stationary blade side of the gas turbine, and a heat shield Although a seal plate or the like disposed between the ring and the ring is a target, in the first embodiment, for example, as shown in FIG. 1, a hollow annular gasket 10A is manufactured. Such a gasket 10A is, for example, as shown in FIG. 2, generally in the form of a flat plate having a predetermined thickness and having a hollow portion 10Aa at the central portion along the thickness direction, that is, a hollow annular shape. It is.
As one mode of use of such a gasket 10A, for example, as shown in FIG. 2, in a gas turbine or the like operated at a high temperature, a first tubular member 21 constituting a piping joint portion 20 through which fluid flows The gasket 10A is used as a seal member for a gas seal with the second tubular member 22.

The whole of the manufacturing process in the first embodiment is shown in FIG. FIG. 3 shows a process including steps that are not necessarily essential.
In the first embodiment, as the preparation step A, the oxide-based ceramic powder 1 and the fiber sheet (fiber assembly) 2A made of non-oxide-based inorganic fibers are prepared.
In the first embodiment, a slurry of an oxide-based ceramic powder is used as a liquid to be impregnated into the fiber assembly in the subsequent impregnation step, and there, ceramic is used as a starting material of the matrix of the ceramic matrix composite. We use powder. However, in the production method of the present invention, the liquid to be impregnated into the fiber assembly in the impregnation step may be a liquid containing an oxide-based ceramic or an oxide-based ceramic material. Therefore, the starting material of the matrix of the ceramic matrix composite is not limited to the powder of the oxide ceramic, and a substance (ceramic material) that produces the oxide ceramic by thermal decomposition or reaction by heating, for example, oxide ceramic precursor It may be a body solution or a metal salt solution for producing an oxide-based ceramic. These points will be explained again later.

As the oxide-based ceramic powder, for example, powder of alumina (Al ₂ O ₃ ) or powder of mullite (3Al ₂ O ₃ · 2SiO ₂ ) can be used, and rare earth silicate powder or stabilized zirconia (ZrO) ₂ ) or the like may be used, and further, two or more of these mixed powders may be used. The average particle size of the oxide-based ceramic powder is preferably about 0.1 to 10 μm. Among these, stabilized zirconia (ZrO ₂ ) is more expensive than alumina etc., but it is particularly excellent in heat resistance, so it is stable when it is desired to increase the heat resistance of the gasket to about 1700 ° C. It is desirable to use fluorinated zirconia (ZrO ₂ ).

Such ceramic powder 1 is suspended in water as a dispersion medium in the slurry preparation container 4 as slurry 5 in FIG. Here, the concentration of the slurry (the volume of the entire ceramic powder relative to the volume of the entire slurry) is preferably 20 to 70 vol%. The dispersion medium of the slurry is not limited to water, and organic solvents such as acetone, benzene, hexane and acetone can also be used. Further, as a dispersion medium for dispersing the ceramic powder, it is also possible to use a solution in which a substance that produces a ceramic by heating, such as a ceramic precursor polymer or a metal salt, is dissolved.
In addition, as a slurry, a dispersion medium such as water, a dispersing agent such as ammonium polycarboxylate for promoting dispersion of ceramic powder, and polyvinyl alcohol so that ceramic powder particles do not fall off at a stage after the later drying step A binder resin such as (PVA) may be added.

On the other hand, as the sheet 2A made of non-oxide inorganic fiber, a fiber aggregate in which short fibers of non-oxide inorganic fiber are randomly intertwined (that is, the directionality of each short fiber is random) is used. Such a fiber assembly is called non-woven fabric or felt. A carbide-based inorganic fiber is typical as the non-oxide-based inorganic fiber, and among them, SiC (silicon carbide) is preferable because of its excellent heat resistance.
The fiber length of the short fibers constituting the fiber assembly of the sheet 2A is not particularly limited, but in general, it is preferably about 1 to 50 mm. Further, the diameter of the short fibers constituting the fiber assembly of the sheet 2 is not particularly limited, but in general, it is preferably about 1 to 10 μm.

A shaping process C is applied to such a sheet 2A (fiber assembly) so as to have a shape corresponding to the final product shape. In the first embodiment, since a hollow annular gasket is manufactured, in the first embodiment, the sheet 2A is processed into a hollow annular shape to form a gasket-shaped sheet 2B. Although the processing means is not particularly limited, a method of punching out the sheet 2A or a method of cutting may be applied.
Depending on the case, the shaping step C may be combined with the impregnation step D described later, and the details of the point will be described in detail in the description of the impregnation step D.

The sheet 2B processed into, for example, a hollow annular shape by the shaping step C is then subjected to the impregnation step D. That is, the shaped sheet 2B is immersed in the slurry 5 in the immersion bath 6 to impregnate the slurry. As a result, the ceramic powder particles in the slurry will intrude into the spaces between the fibers of the sheet 2B.
The sheet 2C thus impregnated with the slurry is then subjected to the drying step E. In order to more fully impregnate the slurry, the impregnation step and the drying step may be repeated twice or more.

  Here, the shaping step prior to the impregnation step may be omitted, and the impregnation step may be performed concurrently with the shaping step. For example, a fiber sheet 2A in which short fibers are irregularly entangled is finely cut, and the many cut fiber pieces are spread in a mold having a gasket shape so as to have a uniform thickness, and slurry May be injected into a mold to impregnate the spread fibers with a slurry to obtain an impregnated sheet 2C having a gasket shape.

  In the drying step E, for example, the impregnated sheet 2C may be inserted into the heating chamber 7 for drying and heated to about 80 to 150 ° C. to evaporate the water in the slurry. The sheet 2D thus dried is then subjected to the firing step F.

  In the first embodiment, the firing step F incorporates the dried gasket-shaped sheet 2D into a device 8 to be operated at a high temperature, for example, a place to be used as a gasket in a gas turbine. And heat the sheet 2D by the heat applied to the gasket shaped sheet 2D during operation. For example, as a seal member for gas seal between the first annular member 21 and the second annular member 22 of the piping joint portion 20 (see FIG. 2) through which high temperature fluid flows in a gas turbine of a real machine The actual machine is assembled in this state, and the gas turbine is operated. At the time of actual operation, the gasket-shaped sheet 2D is exposed to a high temperature of about 900 to 1400 ° C., whereby the sinter bonding of the oxide-based ceramic powder particles (for example, alumina particles) progresses and the non-oxide Sinter bonding progresses between the base inorganic fibers (for example, SiC fibers) and the oxide ceramic powder particles. Therefore, the gasket-shaped sheet 2D becomes a gasket 10A made of a fired ceramic matrix composite material (a composite material in which an oxide ceramic is used as a matrix and fiber reinforced by non-oxide inorganic fibers).

  Here, although the appropriate firing temperature for reliably advancing the firing and causing no problems such as the start of melting of the composite material is generally 900 to 1,400 ° C. although it slightly varies depending on the constituent materials. Therefore, even in the first embodiment, it is desirable to dispose the gasket-shaped sheet 2D at a location exposed to such a temperature during actual operation, but in a large industrial gas turbine, it is exposed to such a temperature range In general, the firing can be sufficiently advanced without causing problems such as melting of the constituent materials. In addition, the actual machine operation time for firing may be at least as long as the progress is completely completed, and generally one hour or more is sufficient.

  A gasket (seal member) manufactured in a state of being incorporated into a high temperature part of an actual machine by the method of the first embodiment is a void portion between fibers in a fiber aggregate consisting of irregularly intertwined non-oxide inorganic fibers And the ceramic and the fiber are sinter-bonded.

Second Embodiment
In the second embodiment, as a seal member to be manufactured, a seal plate 10B interposed between the heat shield ring 31 and the split ring 32 as shown in FIG. 4 on the stationary blade side of a large industrial gas turbine, for example. An example of manufacturing
Conventionally, metal such as heat resistant steel or Ni base super alloy is used as a heat shield ring or split ring in this kind of gas turbine, and a seal plate for gas sealing between the heat shield ring and the split ring It was common to use the same metal as. However, in recent years, attempts have been made to use ceramic matrix composites (CMCs) that are superior in heat resistance and heat insulation to metals as one or both of the heat shield ring and the split ring. In that case, it is also desirable to use a ceramic matrix composite excellent in heat resistance and heat insulation as a seal plate between the heat shield ring and the split ring. However, in the ceramic matrix composite manufactured by applying the conventional general method, it is difficult to secure the sealability. Therefore, in the second embodiment, the manufacturing method of the present invention is applied when manufacturing a seal plate made of this kind of ceramic matrix composite material.

  The process in the manufacturing method of the second embodiment is that the final shape of the seal member is not a gasket shape, but a shape that is disposed as a seal plate between the heat shield ring and the split ring in the gas turbine. The process is different from the process of one embodiment, and the other processes may be similar to the process shown in FIG. Then, before finally firing, the gas turbine is incorporated in a gas turbine of a real machine, and the gas turbine is operated in that state, and firing is performed by heat at the time of operation as in the first embodiment.

<Operation / Effect of First Embodiment, Second Embodiment>
The seal member (gasket or seal plate) manufactured according to the manufacturing method of each of the above embodiments can exhibit excellent sealing performance as compared with a seal member manufactured by a conventional general method. . The reason will be described below in comparison with the seal member according to the conventional method.

  A sealing member in a gas turbine or the like is originally for preventing (sealing) the flow of gas, and in order to ensure sealing performance, between the surface of the sealing member and a mating material with which the sealing member is in contact. It is strongly desirable that the

  However, in a seal member made of a conventional general ceramic matrix composite material, a woven fabric is used as a fiber reinforcing material of the composite material, and since the woven fabric is woven by warp yarns and weft yarns, deformation is attempted. In this case, the degree of freedom of deformation is low because of the large resistance and large in-plane anisotropy. Therefore, when trying to arrange a seal member made of a conventional ceramic matrix composite material in a portion having a complicated shape, ie, a portion where the surface of the mating material is not a simple plane, the deformation resistance is large and the freedom of deformation is low. Therefore, it is difficult to ensure that the seal member conforms to the surface shape of the mating material, and the sealability can not be sufficiently secured. In particular, in the seal plate of the gas turbine to be manufactured in the second embodiment, the surface in contact with the seal plate in the heat shield ring and the split ring, which are counterparts, is often not flat in that case. There is a concern that a gap may be generated between the heat shield ring and the split ring.

  Further, in the ceramic matrix composite material used in the conventional sealing member, it is usual that pores between the fibers are exposed on the surface thereof and fine irregularities are present. Therefore, a space is formed between the mating material and the mating material at the location of the recess on the surface of the seal member, and the sealing performance can not be sufficiently improved.

  On the other hand, in the seal member of the first embodiment and the second embodiment, the fibers as the fiber reinforcement in the composite material are not aligned as warps and wefts, but are entangled randomly, so deformation resistance There is no in-plane anisotropy at the same time, it can be easily deformed (curved, bent, etc.) in any direction. Therefore, even in a portion having a complicated shape, it can be made to closely adhere to the surface of the mating material with certainty along the surface shape of the mating material, and the sealing performance can be secured. In particular, as a seal plate between the heat shield ring of the gas turbine and the split ring, which is the object in the second embodiment, when the surface in contact with the heat shield ring and the split ring in the seal plate has a complicated shape. , The above-mentioned effect can be exhibited effectively.

  In the first embodiment and the second embodiment, the seal member is incorporated in the high temperature region of the actual machine in the unbaked state (the state where only the impregnated sheet is dried), and firing is performed by heat during actual machine operation. There is. At the unbaked stage, hardness and rigidity are much lower than in the fired state, so that it can be easily deformed along the surface shape of the mating material when in an actual machine and sufficiently adhered to the mating material. This is also a factor that can improve the sealability. Also in this respect, the seal plate between the heat shield ring and the split ring of the gas turbine, which is particularly targeted in the second embodiment, has a complicated surface in contact with the heat shield ring and the split ring in the seal plate. In the case of the shape, the above-described effects can be exhibited effectively.

  Furthermore, in the first embodiment and the second embodiment, since the fiber sheet is impregnated with the slurry of the ceramic powder, the pores of the surface of the fiber are also filled with the ceramic powder particles, and as a result, the surface is less uneven. There is little possibility that the void derived from the above-mentioned void is generated between the other material, and this is also a factor which can improve the sealability.

  The mating material with which the sealing member is in contact may be metal or ceramic matrix composite material, but in the case where the mating material is a ceramic matrix composite, the sealing material may be incorporated into the actual machine before firing. By applying the method of the first embodiment or the second embodiment of firing by heat during operation of the actual machine, the adhesion to the partner material can be further enhanced. That is, at the same time as firing, the matrix-constituting material (oxide-based ceramic powder particles) of the seal member is sintered, and at the same time the matrix-constituting material is sinter-bonded also to the ceramic matrix composite material of the mating material. Adhesion to the material is further enhanced. Therefore, as in the case of the second embodiment, when the ceramic base composite material is used for either or both of the thermal barrier ring and the split ring of the gas turbine, the effect is exhibited effectively.

  And the sealing member of 1st embodiment and 2nd embodiment can fully ensure sealing performance combining these effect | actions and effects. Therefore, it is possible to sufficiently secure the sealability necessary for the seal member while making use of the characteristics of the ceramic matrix composite material that the heat insulation is excellent, so that both the heat insulation and the sealability were actually achieved. It has become possible to use it as a seal member for high temperature parts such as high temperature gas turbines.

  With regard to heat insulation, in the first embodiment and the second embodiment, the constituent material of the seal member is a ceramic base composite material, and its thermal conductivity is much lower than that of a metal seal member, and hence a gas turbine Sufficient heat insulation can be exhibited as a seal member used for high temperature parts, such as.

  Further, in the seal member of the first embodiment and the second embodiment, non-oxide inorganic fibers such as SiC are used as a fiber reinforcing material, and non-oxide inorganic fibers of this type are alumina, mullite, etc. It is excellent in heat resistance compared with the oxide-based ceramic of 1. Therefore, the heat resistance can be sufficiently secured as a seal member incorporated in an industrial gas turbine or the like reaching a high temperature of about 1300 to 1400 ° C.

  Furthermore, in the seal plate between the heat shield ring and the split ring in the gas turbine targeted in the second embodiment, one or both of the heat shield ring and the split ring is made of a ceramic base composite material If the seal plate is made of metal, the thermal expansion coefficient of the seal plate metal is larger than that of the ceramic base composite material of the thermal barrier ring or the split ring as the counterpart material, so the thermal expansion difference due to the high temperature during operation causes As a result, the ceramic base composite material of the thermal barrier ring or the split ring may be damaged and the sealing performance may be deteriorated. However, by forming the seal plate also with the ceramic matrix composite material, it is possible to reduce the above-mentioned difference in thermal expansion and to prevent in advance the deterioration of the sealability due to the damage of the thermal barrier ring or the split ring at the time of thermal expansion. It can.

  When the seal plate is made of metal and either or both of the heat shield ring and the split ring is a ceramic matrix composite, the surface hardness at the contact surface is different, so the surface wears out due to vibration during operation. Progress, and there is concern that the sealing performance may be reduced. However, as shown in the second embodiment, the seal plate is also formed of the ceramic matrix composite material, so that it is possible to prevent the deterioration of the sealability due to the progress of the wear.

<Other Embodiments>
In the above description, ceramic powder is used as a starting material for an oxide-based ceramic constituting a matrix of a composite material, a slurry containing the ceramic powder is prepared, and non-oxide based inorganic fibers are randomly selected. The entangled fiber sheet is to be impregnated with the slurry. However, the liquid material to be impregnated into the fiber sheet is basically not limited to the slurry since it may be any one containing an oxide-based ceramic powder or an oxide-based ceramic material.
For example, the above-mentioned liquid is a solution containing an oxide-based ceramic precursor or a metal salt for forming an oxide-based ceramic as a substance (ceramic material) that produces an oxide-based ceramic by thermal decomposition or reaction by heating. It is also good. Examples of the oxide-based ceramic precursor include aluminum alkoxide and zirconium alkoxide, and examples of the metal salt include aluminum chloride and zirconium chloride.

  Furthermore, in the first embodiment and the second embodiment, they are incorporated into a high temperature part such as a gas turbine of a real machine at the stage before firing, and are heated and fired by the operation of the real machine. It is also acceptable to carry out the firing step at a stage prior to installation in a real machine. As baking conditions in that case, it is preferable to set it as 900-1400 degreeC for 1 hour or more.

  Examples of the present invention will be described below. The following examples are examples for verifying the effects of the present invention, and it is a matter of course that the conditions of the examples do not limit the scope of the present invention.

Example 1:
A fine-grained alumina powder (made by Daimei Kagaku: TM-DAR) having an average particle diameter of 0.16 μm is prepared as an oxide-based ceramic powder, and a 10-mm-thick fiber sheet (fiber aggregate) made of non-oxide inorganic fibers And felt made of short fibers of SiC. The average fiber length of the SiC short fibers constituting the felt is 10 mm, the average fiber diameter is 10 μm, and the porosity of the felt is about 90%.

  100 g of the above-mentioned fine particle alumina powder was added to 80 g of distilled water together with 2 g of a dispersing agent (manufactured by Chukyo Yushi Co., Ltd .: Celna D 305) and 5 g of PVA as a binder to form a slurry. On the other hand, the above felt was processed into a gasket shape (hollow ring) by punching. The processed felt was impregnated with the slurry to form an impregnated sheet. The slurry after slurry impregnation was heated to 80 ° C. and dried.

  The sheet having the gasket shape after drying was attached to a pipe joint location through which high temperature gas in an actual gas turbine flows, and the gas turbine was actually operated in that state. It is estimated that the gasket-shaped sheet in operation is heated to about 900 to 1400 ° C.

  After applying a heat history equivalent to one hour or more in a real machine, a pressure resistance test was conducted in a normal temperature environment to check the sealability. As a result, it was confirmed that the seal was ensured. From this, it is estimated that the gasket-shaped sheet is sufficiently fired at the time of actual machine operation.

Example 2:
An aluminum isoproxide (made by Showa Chemical Co., Ltd.) is prepared as an oxide-based ceramic forming material, and a 10 mm thick felt made of SiC short fibers is prepared as a fiber sheet (fiber assembly) made of non-oxide inorganic fibers. did. The average fiber length of the SiC short fibers constituting the felt is 10 mm, the average fiber diameter is 10 μm, and the porosity of the felt is about 90%.

  40 g of the above-mentioned aluminum isopropoxide was added to 80 g of hexane to form a raw material solution (liquid). On the other hand, the above felt was processed into a gasket shape (hollow ring) by punching. The raw material solution was impregnated into the processed felt to make an impregnated sheet. The impregnated sheet was dried by heating to 80.degree.

  The gasket-shaped sheet after drying was attached to a pipe joint or the like through which high-temperature gas flows in a real gas turbine, and the gas turbine was actually operated in that state. It is estimated that the gasket-shaped sheet in operation is heated to about 900 to 1400 ° C.

  After applying a heat history equivalent to one hour operation in a real machine, the pressure resistance test was conducted in a normal temperature environment and the sealability was examined. As a result, it was confirmed that the seal was surely performed. From this, it is estimated that the gasket-shaped sheet is sufficiently fired at the time of actual machine operation.

Example 3:
Aluminum chloride hexahydrate powder (manufactured by Wako Pure Chemical Industries, Ltd.) is prepared as an oxide-based ceramic-forming material, and a thickness of short fibers of SiC as a fiber sheet (fiber assembly) made of non-oxide-based inorganic fibers A 10 mm felt was prepared. The average fiber length of the SiC short fibers constituting the felt is 10 mm, the average fiber diameter is 10 μm, and the porosity of the felt is about 90%.

  40 g of the above aluminum chloride hexahydrate powder was added to 100 g of distilled water to form a raw material solution (liquid). On the other hand, the above felt was processed into a gasket shape (hollow ring) by punching. The raw material solution was impregnated into the processed felt to make an impregnated sheet. The impregnated sheet was dried by heating to 80.degree.

  The gasket-shaped sheet after drying was attached to a pipe joint or the like through which high-temperature gas flows in a real gas turbine, and the gas turbine was actually operated in that state. It is estimated that the gasket-shaped sheet in operation is heated to about 900 to 1400 ° C.

  After applying a heat history equivalent to one hour operation in a real machine, the pressure resistance test was conducted in a normal temperature environment and the sealability was examined. As a result, it was confirmed that the seal was surely performed. From this, it is estimated that the gasket-shaped sheet is sufficiently fired at the time of actual machine operation.

  Although the preferred embodiments and examples of the present invention have been described above, these embodiments and examples are merely examples within the scope of the present invention and do not depart from the scope of the present invention. Configuration additions, omissions, substitutions, and other changes are possible. That is, the present invention is not limited by the above description, and is limited only by the appended claims, and it is needless to say that the present invention can be appropriately modified within the scope.

1 ceramic powder 2 fiber sheet (transition aggregate)
2B impregnated sheet (impregnated body)
5 Slurry (solvent)
10A gasket (seal member)
10B Seal plate (seal member)
D Impregnation process F Baking process

Claims (8)

An impregnating step of impregnating a fiber assembly comprising non-oxide inorganic fibers randomly intertwined with an oxide-based ceramic powder or a liquid containing an oxide-based ceramic material to form an impregnated body;
And a firing step of firing the impregnated body.   The manufacturing method of the sealing member for high temperatures of Claim 1 whose said non-oxide type inorganic fiber is a SiC type fiber.   The method for producing a high temperature sealing member according to any one of claims 1 and 2, wherein a slurry in which an oxide ceramic powder is suspended in a dispersion medium is used as the liquid in the impregnation step. .   The sealing member for high temperature according to any one of claims 1 and 2, wherein an oxide-based ceramic precursor solution or a metal salt solution for forming an oxide-based ceramic is used as the liquid in the impregnation step. Manufacturing method. The above-mentioned impregnated body is disposed at the place where the seal member in the actual machine is to be attached, at a stage before the firing step
The manufacturing method of the sealing member for high temperatures as described in any one of Claims 1-4 which heats an impregnated body by the heat added to the said impregnated body at the time of driving | operation of a real machine as said baking process.   The method for manufacturing a high temperature sealing member according to any one of claims 1 to 4, wherein the firing step is performed at a stage before mounting on a real machine as a high temperature sealing member of a product. The method for manufacturing a high temperature sealing member according to claim 1, wherein the high temperature sealing member is a member used for a gas turbine.   A fiber assembly composed of irregularly intertwined non-oxide inorganic fibers, characterized in that an oxide-based ceramic is filled in spaces between the fibers, and the fibers and the ceramic are sinter-bonded. High temperature sealing member.

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