JPH11255567A - Ceramic fiber-combined material part and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a ceramic fiber-combined material part capable of forming holes with continuous fibers without applying a mechanical processing, capable of lowering the cost of production and capable of improving the reliability of the part by allowing the holes formed in a pre-form at a stage for forming the pre-form of fibers to exist after the formation of the combined material part which has the holes in the constituting wall. SOLUTION: Fibers are wound on a core 1 so as to uniformly share a stress in an axial direction and in a circumferential direction. Fibers 5 oriented at an angle of 67.5 degree and fibers 6 oriented at an angle of 22.5 degree are especially alternately wound by a filament-winding method to form three layers, respectively, around each circular hole 4 in which a pin 2 is inserted. The fibers are wound at the oriented angles to obtain the pre-form. When the wound fiber arrangement around the circular hole 4 is two-dimensionally looked, the wound fiber arrangement has an uniform pattern, and the portion around the circular hole 4 is densely formed without having a coarse fiber portion. While the holes 4 are maintained, the formed pre-form is combined with a matrix material to form a cylindrical combustor liner, etc.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a silicon carbide (Si)
C) A technique related to a ceramic fiber composite material component in which ceramic fibers are composited in a matrix and a method for manufacturing the same. The cylindrical shape is particularly applied to a combustor liner and the like, and has high strength and high strength even in a high temperature region. The present invention relates to a ceramic fiber composite material part having excellent toughness and oxidation resistance and reduced cost, and a method for producing the same.

[0002]

2. Description of the Related Art Composite materials in which various long fibers composed of inorganic materials, organic materials, and metallic materials are compounded in a matrix such as resin, metal, or ceramics are mechanically compared with monolithic materials in which no composite is formed. Due to improvements in properties and physicochemical properties, research and commercialization thereof have been promoted in various industrial fields and living fields.

[0003] In particular, a fiber reinforced plastic (FRP; fibre) obtained by compounding a plastic with carbon fiber or glass fiber.
The ber reinforced plastic has characteristics that the composite fiber has excellent high elastic modulus and high strength characteristics and is lightweight. For this reason, fiber-reinforced plastic is used as a component of industrial products such as aircraft, ships, and automobiles, as well as in sports equipment such as skis, tennis racket frames, golf club shafts and fishing rods, and in entertainment-related parts. Has also been widely used.

In recent years, the development of fiber composite materials in which ceramic-based long fibers are compounded in a metal or ceramic sintered body has been widely promoted. A specific example is a carbon matrix composite material reinforced with carbon fibers. This carbon matrix composite material is used as a high-temperature molding material or a heat-resistant structural part of a space shuttle, because its specific strength, which is the strength per unit amount in a high temperature range, is particularly large.

Further, structural parts used for gas turbine parts, aircraft parts, and automobile parts are required to have high reliability in addition to strength in a high temperature range. To ensure high reliability, the fracture toughness and fracture energy value,
And ceramic-based composite materials with improved impact resistance (CM
Research into the practical use of C; ceramic matrix composite) components and metal matrix composite (MMC) components is underway during internal and external research periods. These ceramic-based composite materials and metal-based composite materials are manufactured by dispersing and complexing composite materials such as fibers, whiskers, plates, and particles made of inorganic substances and metals in a matrix.

[0006] In the above-mentioned composite material, if the material to be dispersed and composited in the matrix is a long fiber, the effect of improving the mechanical properties becomes particularly large. In this case, in order to improve the mechanical properties, it is necessary to compound a relatively large amount of fibers in the matrix.

[0007] In order to make a composite material into a three-dimensional structure, a long fiber to be dispersed and compounded in a matrix is previously woven or laminated in two-dimensional and three-dimensional directions or laminated to form a preform. It is necessary to form a fibrous structure. Then, it is possible to produce a three-dimensional structure by impregnating the matrix with the fibrous structure.

However, the conventional fiber composite material in which a fiber structure composed of various long fibers is compounded in a matrix has a drawback that the strength characteristics of the composite material are anisotropic due to various orientation angles of the fibers. there were. For this reason, for example, when thermal stress is considered to act equally in the axial direction and the circumferential direction in the combustor liner, if the fiber is not oriented at 45 degrees with respect to the axis, the isotropic Material could not be obtained.

Further, in a combustor liner or the like having a cylindrical shape, holes such as an ignition hole and an air intake hole are provided in a direction perpendicular to the axis of the combustor liner. It was formed by processing.

[0010]

However, the ceramics constituting the matrix of the composite material or the ceramics constituting the composite long fiber described above are extremely brittle and have high hardness, so that the composite material component is not mechanically machined. In order to form a hole by machining, costly methods such as ultrasonic machining and electric discharge machining have to be taken, which is economically problematic.

[0011] Even after machining by such ultrasonic machining and electric discharge machining, the cut fibers are exposed at the end faces of the holes. In an environment exposed for a long time, oxidation may proceed from the cut portion of the hole end surface.
For this reason, in order to protect the cut surface, there is a method of forming an oxidation resistant film by chemical vapor deposition (CVD), but this also leads to a significant increase in cost and economical. There was a problem.

[0012] For this reason, when attempting to form holes with continuous fibers without machining, it is necessary to arrange the fibers so as to bypass the periphery of the holes. In fact, to form the holes with continuous fibers, it is possible to deliberately bypass the fibers by setting up a pin at the position where the holes of the preform weaving core are to be formed. However, due to the rigidity of the fiber itself, the fiber does not bend along the periphery of the hole and is arranged avoiding the hole so as to pass through the tangent to the outer periphery of the hole. Will not be arranged. For this reason, when an external impact is applied to the part where the fiber is not arranged,
There has been a problem that catastrophic destruction may occur as in the case of monolithic ceramics in which various materials are not compositely dispersed, and high reliability cannot be obtained.

SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problem, and it is possible to reduce costs and obtain high reliability by forming holes with continuous fibers without performing machining. It is an object of the present invention to provide a method for manufacturing a ceramic fiber composite material part.

Among ceramic-based composite materials, a composite material using SiC as a matrix having high heat resistance has attracted attention, especially when considering its application as a high-temperature material. , C
VI (Chemical Vapor Infiltration) method, PIP (Polym
er Impregnation Pyrorysis) method and reaction sintering method. Among these, the reaction sintering method is a matrix synthesis technique applicable to high-temperature structural members having high matrix denseness, high initial fracture strength characteristics, and excellent heat resistance and long-term stability.

The formation of the matrix by the reaction sintering method is as follows.
The fiber preform is impregnated with SiC and C as a matrix component, and the impregnated fiber preform is melted with Si.
To form a dense SiC matrix by reacting C and Si.

When the impregnation of the matrix component is considered for a cylindrical article, a slurry casting method is generally used. In the slurry casting method, a porous mold having holes (cavities) of a structure to be formed is used, and a slurry in which powder and water serving as a matrix component are dispersed is poured into the cavity, and a capillary is formed in the porous mold. This is a method in which moisture is absorbed by utilizing the phenomenon, and a powder serving as a matrix component is deposited on the surface of the porous mold to obtain a structure. As a method of considering mold release after molding, as a method for a cylindrical object, a porous columnar core and an outer mold (case body) divided into a plurality of parts maintaining the same shape as the outer diameter of the structure Is formed by pouring the slurry into the cavity formed between the core and the outer mold. In the case of ceramic fiber composites, impregnation and molding of the matrix inside the fiber preform is possible.

However, when the preform is inserted between the core and the outer mold, the slurry is difficult to penetrate and impregnate into the interior due to a small gap between the cavities, and the impregnation is partially insufficient. There is a problem that the slurry is impregnated and deposited at the periphery of the slurry inlet, and the slurry is blocked and does not permeate into the inside. When the impregnated preform partially impregnated with the matrix component is impregnated with molten Si as described above, since there is no C that reacts in the portion where the impregnation of the matrix component is insufficient, a Si-rich matrix is formed. Therefore, there is a problem that the matrix becomes non-uniform.

The present invention has been made in order to solve the above-mentioned problems. In manufacturing a ceramic fiber composite material part, a reaction sintering method is used. An object of the present invention is to provide a ceramic fiber composite material part which can obtain a uniform and dense matrix by applying pressure, and can secure high strength, high toughness and oxidation resistance even in a high temperature region.

[0019]

According to a first aspect of the present invention, there is provided a ceramic fiber composite material component comprising a ceramic matrix and fibers.
The hole formed in the preform at the stage of forming the fiber preform is left after compounding, so that the constituent wall has a hole.

In the present invention, it is possible to greatly reduce the cost by obtaining a structural wall having holes by fibers without performing machining for forming the holes.

A ceramic fiber composite material component according to a second aspect is the ceramic fiber composite material component according to the first aspect, wherein the composite fiber is a continuous fiber, and the formed article after the composite is formed by a plurality of orientation angles of the continuous fiber. It is a cylindrical shape formed by laminating, and the hole in the structural wall is a gap formed in the laminated portion of the continuous fiber.

In the present invention, the cylindrical structural wall having holes is formed by arranging reinforcing fibers in a ceramic matrix, and the reinforcing fibers have a structure in which fibers are laminated at a plurality of orientation angles. . Further, by combining fibers having a plurality of orientation angles, it is possible to increase the fiber density around the hole without cutting the fibers.

Further, in the present invention, the present inventors have attempted to obtain a cylindrical preform having holes by various preform forming methods. As a result, it was possible to obtain a preform having holes by combining continuous fibers with not only fibers having a single orientation angle but also fibers having a plurality of orientation angles by a filament winding method or a braiding method.

The ceramic fiber composite material component according to claim 3 is the ceramic fiber composite material component according to claim 1 or 2, wherein the orientation angles of the continuous fibers are θ1, θ2,.
When θn is set, the axial stress component (Cos ² θ1 + C
os ² θ2 +... θn) and the circumferential stress component (Sin
² θ1 + Sin ² θ2 +... Θn)

(Equation 3) It is characterized by having.

In the present invention, when a fibrous structure is obtained at an orientation angle θ, the axial stress component / circumferential stress component is expressed by C
os ² θ / Sin ² θ, the axial stress component / circumferential stress component in a laminate having orientation angles θ1, θ2,. Is (Cos ² θ1 + Cos ² θ2 + θn) / (Si
^{n 2 θ1 + Sin 2 θ2 +} ·· θn) to become. Therefore,
By setting the ratio of the axial stress component / circumferential stress component to 1, a structure capable of sharing an even stress can be obtained, and a preform having holes can be formed of continuous fibers.

According to a fourth aspect of the present invention, there is provided a ceramic fiber composite material part according to any one of the first to third aspects, wherein a silicon carbide ceramic formed by a reaction sintering method is used as a ceramic matrix. It is characterized by being applied.

In the present invention, silicon carbide (S) formed by a reaction sintering method is used as a ceramic matrix.
By using iC) ceramics, a uniform and dense matrix can be obtained, and a ceramic fiber composite material component having high strength, high toughness and oxidation resistance even in a high temperature region can be obtained.

According to a fifth aspect of the present invention, there is provided a ceramic fiber composite material part according to any one of the first to fourth aspects, wherein the continuous fiber comprises a fiber body mainly composed of silicon carbide and the fiber body. And an interface layer covering at least one of at least one material selected from boron nitride, silicon carbide and carbon, and having a thickness of 0.1 to 2 microns. It is characterized by being.

In the present invention, the interface layer covering the surface of the fiber main body is made of boron nitride (BN), silicon carbide (SiC).
And at least one of carbon (C) and S
It is preferably an iC-based fiber. As this interface layer, a sliding layer having a thickness of 0.1 to 2 microns is preferably formed. This sliding layer is introduced for the purpose of preventing the fibers and the matrix from being firmly bonded to each other. The sliding layer easily exhibits a combined effect of bridging and pull-out (pull-out), and has an effect of preventing brittle fracture. .

In particular, the boron nitride (BN) layer has a function of weakening the bond between the fiber and the matrix, causing the fiber to be pulled out when broken, and
The layer (C) has a function of preventing an interfacial reaction between the fibers and the matrix when the matrix is formed.

In the present invention, the slip layer is formed in a thickness range of 0.1 to 2 microns. However, when a preform is formed by a filament winding method or a braiding method, the fiber surface is rubbed by the fibers. This is because the slipping layer may peel off, and the tendency becomes severe at 2 μm or more. Due to the separation of the sliding layer, a portion where the matrix and the fiber are firmly bonded appears, and as a result, it is difficult to exhibit an effective composite effect. On the other hand, when the sliding layer has a thickness of 0.1 μm or less, the effect is weak, and the matrix and the fiber are strongly bonded as a whole, so that it is difficult to exhibit the composite effect. Therefore, in the present invention, it is desirable to form the sliding layer with a thickness in the range of 0.1 to 2 microns.

According to a sixth aspect of the present invention, there is provided a method of manufacturing a ceramic fiber composite material component in which a ceramic matrix and a fiber are combined, wherein the fibers are laminated to form a preform having holes. Thereafter, the preform is impregnated with a ceramic matrix slurry to obtain a molded body. Thereafter, the matrix slurry is dried and sintered, and is integrated with the preform to form a cylindrical body having holes in a structural wall. It is characterized by manufacturing parts.

In the present invention, by forming a preform having holes using fibers, the structural wall can be manufactured without machining, thereby reducing the cost.

According to a seventh aspect of the present invention, there is provided a method of manufacturing a ceramic fiber composite material part according to the sixth aspect, wherein continuous fiber is used as the composite fiber, and the continuous fiber is formed at a plurality of orientation angles. It is characterized in that a preform is formed by laminating the fibers so that the gap between the fibers is a hole.

In the present invention, a cylindrical structural wall having holes can be formed by laminating continuous fibers at a plurality of orientation angles. In particular, when a uniform stress is generated around the hole, a structural wall capable of uniformly sharing the stress generated around the hole can be obtained by controlling the fiber orientation angle.

Specifically, the oriented fibers of the preform are:
More preferably, the fibers are oriented so that the angles formed by the oriented fibers are equiangular. Here, the angle formed by the oriented fibers is equal, for example, a combination of oriented fibers of 0 degree and 90 degrees, a combination of 22.5 degrees and 67.5 degrees, and 0 degrees.
The angles formed by the oriented fibers are 90 degrees, 45 degrees, 45 degrees, and 30 degrees, respectively, such as a combination of degrees, 45 degrees, and 90 degrees, and a combination of 15 degrees, 45 degrees, and 75 degrees. When viewed on a two-dimensional plane, the fiber arrangement around the hole becomes a uniform pattern, and as a result, this structure creates a structural wall that has a structure that can equally share the stress acting in the circumferential direction and axial direction. Can be manufactured.

The method for producing a ceramic fiber composite material component according to claim 8 is the method for producing a ceramic fiber composite material component according to claim 6 or 7, wherein the orientation angles of the continuous fibers are θ1, θ2,. , The axial stress component (Cos ² θ1 + Cos ² θ2 +... Θn)
Circumferential stress component (Sin ² θ1 + Sin ² θ2 +
· Θn)

(Equation 4) It is characterized by the following.

In the present invention, the orientation angles θ1, θ2,.
When a fibrous structure is obtained from a laminated body of θn (thickness of each layer and the number of laminated layers are assumed to be the same), by setting the axial stress component / circumferential stress component to 1, a structure capable of sharing even stress is obtained. And the structural wall having holes can be formed of continuous fibers.

According to a ninth aspect of the present invention, there is provided a method for manufacturing a ceramic fiber composite material part according to any one of the sixth to eighth aspects, wherein a plurality of monofilaments are bundled as a composite fiber to obtain a fiber. Using a continuous fiber as a bundle, a cylindrical preform having holes with the continuous fibers is formed, and the formed body is dried and degreased, and then fired by a reaction sintering method to form a cylindrical part having holes in a structural wall. It is characterized by obtaining.

In the present invention, a preform is formed by using a fiber bundle formed by bundling a plurality of monofilaments, and the obtained preform is impregnated with a matrix slurry to form a formed body. The obtained formed body is degreased and dried. By integrating the matrix and the fiber by the reaction sintering method, it is possible to obtain a ceramic fiber composite material part having a dense structure wall.

According to a tenth aspect of the present invention, there is provided a method of manufacturing a ceramic fiber composite part according to any one of the sixth to ninth aspects.
By inserting the preform into a core made of a porous material, immersing the preform in a matrix slurry in a slurry container in this state, and reducing the pressure through an exhaust port arranged at the upper end portion of the slurry container of the core. And depositing the matrix slurry on the preform.

For the impregnation of the matrix slurry, the preform is inserted into a porous core, and is immersed in the matrix slurry in this state. An exhaust port is arranged at the upper end portion of the core slurry container, and the pressure is reduced by the exhaust port so that the matrix slurry is deposited and the matrix slurry can be impregnated from the entire surface of the preform.

According to the present invention, partial impregnation can be prevented from being insufficient, and a uniform and dense matrix can be obtained.

In the method for manufacturing a ceramic fiber composite material component according to the eleventh aspect, in the method for manufacturing a ceramic fiber composite material component according to the tenth aspect, the matrix slurry may be supplied from the outside of the slurry container at a pressure of liquid or gas pressure of 0.1. ~
It is characterized in that pressure is applied in the range of 30 MPa.

In the present invention, the impregnation of the matrix slurry is preferably performed by pressurizing the matrix slurry with a liquid pressure or a gas pressure in a range of 0.1 MPa to 30 MPa. When the matrix slurry is impregnated by depressurization, only the fibers on the outer surface of the preform in contact with the surface of the matrix slurry are impregnated, but the fibers inside the preform are not easily impregnated. By applying pressure, it easily penetrates and impregnates inside. The reason why the pressurizing pressure is set to 30 MPa or less is that if the pressure exceeds 30 MPa, the porous core may be broken, and if the pressure is less than 0.1 MPa, the effect is low and the impregnation property is improved. Because there is no.

The method of manufacturing a ceramic fiber composite material component according to claim 12 is the method of manufacturing a ceramic fiber composite material component according to claim 6 or 11, wherein the core is inserted when the preform is impregnated with the matrix slurry. The outer surface of the reform is covered with a case body having a shape similar to that of the preform and having a through hole for permeating the matrix slurry in a wall thereof.

In the present invention, a case body is attached to the outer surface of the preform to cover the inlaid surface of the preform, and a through-hole is formed in the case body to limit the amount of matrix inlaid. There is. According to this molding method, the thickness of the matrix component can be controlled by the case body, and further deposition can be prevented. In addition, the inner surface of the case body is coated with a coating with excellent release properties such as silicone rubber to improve the release properties with the matrix.
Workability can be improved.

[0048]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of a ceramic fiber composite material part and a method of manufacturing the same according to the present invention are shown in FIG.
This will be described with reference to FIGS.

In the present embodiment, a preform having holes with different fiber orientation angles is formed, and a matrix material is compounded while maintaining the holes to form a combustor liner having a cylindrical shape. Will be described.

FIG. 1 is a process chart schematically showing a manufacturing procedure.

As shown in FIG. 1A, a SiC-based fiber was used as a composite fiber, and a BN coat and a SiC coat were double coated on the surface of the fiber as an interface layer with a matrix by a vapor deposition method. Then, as shown in FIG. 1 (B), the fibers were woven into a part shape to form a preform which was a fiber woven body. Then, using a slip pressure impregnation device shown in FIG.
An aqueous matrix slurry composed mainly of (carbon) and SiC powder was injected at high pressure to obtain a molded body.

After the molded body thus obtained is dried, as shown in FIG. 1 (D), it is impregnated with molten Si (silicon) and reacted with C in the molded body to synthesize SiC. After sintering, a combustor liner made of a SiC-based composite material was obtained.

In the present embodiment, Hynicalon (trade name) manufactured by Nippon Carbon Co., Ltd. was used as the SiC-based fiber material. This fiber material was composed of monofilaments having an average diameter of 12 microns, and a yarn obtained by converging 500 monofilaments was used as a continuous fiber. On the monofilament, the BN coat of 0.4 μm and the SiC coat of 0.3 μm were applied in the step of FIG.

FIG. 2 shows a method of manufacturing a preform having a circular hole in the step of FIG.
It is a figure which shows the core used in order to obtain a molded object in the process. That is, the core is used as a bobbin for winding the fiber, and is disposed in the preform at the time of impregnation with the slurry and used for forming the inner surface.

As shown in FIG. 2, the core 1 is made of a porous material such as gypsum. The core 1 is used as a bobbin for winding fibers, and is used as an impregnation core 1a which is arranged in a preform and is used for forming an inner surface during slurry impregnation, and is used as a bobbin for winding fibers. The winding core 1b is sometimes cut, and the impregnating core 1a and the winding core 1b are connected at the center to form an entasis shape.

On the outer surface of the impregnating core 1a, a pin 2 for bypassing the fiber for forming a circular hole is inserted.
A shaft 3 was attached to the end face of the impregnating core 1a. The shaft 3 was rotated by the filament winding method, and the fiber was wound by fixing the shaft 3 by the braiding method.

FIG. 3A is an external view showing an example of the fiber arrangement of the preform, and FIG. 3B is a fiber orientation angle around the circular hole of the preform shown in FIG. 3A. It is a conceptual diagram for demonstrating.

As shown in FIGS. 3A and 3B, the core 1 shown in FIG. 2 was used to wind fibers so that stress could be equally distributed in the axial direction and the circumferential direction. Particularly, around the circular hole 4 into which the pin 2 is inserted, the 67.5-degree oriented fibers 5 and the 22.5-degree oriented fibers 6 are alternately wound by three layers by the filament winding method. A preform was obtained by winding the fiber at such an orientation angle.

As shown in FIG. 3B, when the fiber detour around the circular hole is viewed two-dimensionally, it has a uniform pattern, and the periphery of the circular hole 4 is densely formed without coarse portions. Have been.

FIG. 4A is a view showing another example of the fiber arrangement of the preform, and FIG. 4B is a view of the fiber arrangement around the circular hole 4.

As shown in FIGS. 4A and 4B, the core 1 shown in FIG. 2 was used to wind a fiber so that stress could be equally distributed in the axial direction and the circumferential direction. In particular, around the circular hole 4, fibers having three orientation angles of 75-degree oriented fiber 7, 45-degree oriented fiber 8 and 15-degree oriented fiber 9 were sequentially wound in two layers by a filament winding method. A preform was obtained by winding the fiber at such an orientation angle.

As shown in FIG. 4B, also in this example, there is no coarse portion around the circular hole 4 and the fiber is densely formed.

For comparison, preforms were formed with different fiber arrangements.

FIG. 5 (a) is a diagram showing a comparative example of the fiber arrangement of the preform, and FIG. 5 (b) is a view of the fiber arrangement around the circular hole 4.

As shown in FIGS. 5 (a) and 5 (b), using the core 1 shown in FIG. 2, four layers of 45 ° oriented fibers 10 were wound by a filament winding method to obtain a preform.

As shown in FIG. 5B, unlike the above example, there is a void 11 around the circular hole 4 where no fiber is arranged.

Each of the preforms shown in FIGS. 3 to 5 obtained as described above was cut at the joint between the impregnating core 1a and the winding core 1b. Using the impregnation core 1a thus obtained, the core 1a was impregnated with a matrix slurry as shown in the slip pressure impregnation step of FIG. 1 (c).

The matrix slurry was made of SiC powder (7
(0 wt%) and carbon black (30 wt%) as solids, pure water and a surfactant were added so that the slurry concentration became 50%, and the mixture was mixed with a pot roller for 24 hours. . Then, the matrix slurry was pressure-impregnated into the preform using gas pressure or liquid pressure as described below.

FIG. 6 is a schematic view showing a matrix impregnation method using gas pressure.

As shown in FIG. 6, a closed container 12 with a lid is provided.
The matrix slurry 13 was housed in the container, and the preform 14 was immersed in the matrix slurry 13 together with the core for impregnation 1a. In this case, preform 1
Reference numeral 4 denotes an outer mold 15 to be described later, which covers the outer surface and is entirely immersed in the matrix slurry 13.

The upper end of the impregnation core 1a has an exhaust port 15c.
And the closed container 1 connected to the exhaust port 15c.
(2) Vacuum was drawn by an external vacuum pump 16. The interior of the sealed container 12 is connected to a compressor 17.
The inside of the sealed container 12 was pressurized at 8 MPa, thereby impregnating the preform 14 with the matrix component.

FIG. 7 is a schematic view showing a method of impregnating a matrix by hydraulic pressure.

As shown in FIG. 7, in this method, the inside of the closed container 12 with a lid is partitioned into a double space by a flexible rubber partition 18, and oil 19 is filled between the closed container 12 and the partition 18. Meanwhile, the matrix slurry 13 was accommodated in the partition wall 18. The preform 14 was immersed in the matrix slurry 13 together with the impregnation core 1a. Also in this case, the outer surface of the preform 14 is covered with an outer mold 15 described later, and
3 soaked.

The upper end of the impregnation core 1a has an exhaust port 15c.
And the closed container 1 connected to the exhaust port 15c.
(2) Vacuum was drawn by an external vacuum pump 16. The side surface of the sealed container 12 is connected to a compressor 17, and the compressor 1
7, the oil 19 in the closed container 12 was pressurized at 8 MPa. By this pressurization, the partition wall 18 was contracted and the matrix slurry 13 housed therein was pressurized, and the preform 14 was impregnated with the matrix components.

FIG. 8 is a schematic view showing an outer mold 15 for limiting the amount of inlaid material during matrix impregnation.

As shown in FIG. 8, the outer mold 15 is for controlling the thickness of the matrix formed on the outer surface of the preform 14, and this outer mold 15 is a pair of outer molds 15.
a and the outer mold 15b. The outer mold 15a is composed of a metal case body 20a and a silicone rubber cushioning material 21a coated on the inner peripheral surface of the case body 20a. Similarly, the outer mold 15b is made of a metal case body 2a.
0b and a cushioning member 21b made of silicone rubber coated on the inner peripheral surface of the case body 20b.
On the outer peripheral surface of these case bodies 20a, 20b, holes 22a, 22b for matrix slurry permeation are respectively provided.

The pair of outer dies 15a and 15b has a structure that can be fitted at the central portion, and has a structure in which the impregnation core 1a can be housed inside.

The outer mold 15 having such a structure is impregnated with the core 1 for impregnation.
6A, the impregnating core 1a covered with the outer mold 15 was impregnated into the matrix slurry 13 to obtain a molded body (not shown).

Thereafter, the molded body was taken out of the sealed container 12, dried for a whole day and night, and then the outer mold 15 was removed. Further, the impregnation core 1a and the molded body were separated from each other, and the molded body was degreased. Then, after maintaining in a vacuum state at a temperature of 1450 ° C. for 3 hours, molten Si is impregnated at a temperature of 1450 ° C. for 1 hour under Ar pressure of 0.5 MPa to obtain a SiC-based long fiber composite material part. A combustor liner was obtained.

A peripheral portion of the circular hole 4 of the combustor liner thus obtained was cut out to obtain a test piece, and a thermal shock test was performed.

A test piece of a combustor liner having a fiber orientation of 22.5 degrees to 67.5 degrees shown in FIG. 1
The test piece of the combustor liner having the fiber orientation of 15 ° -45 ° -75 ° shown in FIG. And 2. Further, a test piece of a combustor liner having a fiber orientation of 45 degrees and a single orientation angle shown in FIG. It was set to 3.

The thermal shock test was conducted in a sample No. 1 to No. 3 was carried out by heating and forcibly dropping it into water. Test temperature is 300 ° C, 400
C., 500.degree. C., 700.degree. C., and 900.degree. C., the test piece was heated for 15 minutes under each condition, and then dropped in water.

The sample No. after the thermal shock test was used. 1 to N
o. For No. 3, the degree of damage was confirmed by an appearance inspection and a fluorescence inspection (PT) inspection. Table 1 shows the results. Cracks indicate that cracks were observed by a fluorescent flaw detection (PT) test, while chips indicate that the material was clearly destroyed at a visual level.

[0084]

[Table 1]

As shown in Table 1, the sample No. 1 to No.
No damage was found in the material in the thermal shock test under water from 300 ° C. in all three samples, but the sample No. 3 was used for comparison. For a 45 ° oriented product of No. 3, at a temperature of 400 ° C. or more,
Peeling of the material was observed at a visual level. Especially,
The exfoliated portion is a portion where no fiber exists around the circular hole, and the same destruction as that of the monolithic material occurred because the composite effect by the fiber was not observed.

[0086] Also, in the fluorescence inspection test, cracks extending radially from the circular holes were observed. Sample No. 1 of 2
2.5 ° -67.5 ° oriented product and Sample No. 2 in 15
In the thermal shock test from 900 ° C., no destruction at a visual level was observed for the oriented product of −45 ° to 75 °.
According to the fluorescent flaw detection test, the sample No. In the case of Sample No. 1, the sample No. In No. 2, cracks extending radially from the circular hole of the material at 500 ° C. or higher were observed. The cracks grew longer as the heat treatment temperature increased, but the growth stopped inside the material.

Further, when cracks were observed with a scanning electron microscope, it was observed that the fibers were bridging and pull-out, and that they acted to hinder the progress of cracks.

Therefore, according to the present embodiment, it was found that a material part having excellent flaw detection tolerance can be obtained by forming the circular holes 4 with multi-oriented fibers.

Hereinafter, in the present embodiment, the thickness of the sliding layer coated on the monofilament surface is 0.1 to 2
A description will be given of what is defined as a micron. Specifically, as shown in Table 2, the film thickness was changed and compared.

[0090]

[Table 2]

As shown in Table 2, as shown in FIG. 1 to No. The test materials up to 4 were coated on the monofilament surface with a film thickness ranging from 0.1 to 2 microns.

Specifically, the test material No. 1 was a 1.0 micron BN layer as a coating on the monofilament surface. Test material No. 2 was a 0.4 micron BN layer and a 0.4 micron SiC layer as a coating on the monofilament surface. Test material No. 3
Are used as coatings on the monofilament surface.
There were a 0 micron BN layer and a 0.4 micron SiC layer. Test material No. 4 shows a 1.0 micron BN layer and 0.4
A micron SiC layer was obtained.

In order to make a comparison, No. 5 and No. 5 The test material of No. 6 had a film thickness outside the range of 0.1 to 2 microns.

Specifically, the test material No. 5 was a 1.0 micron BN layer and a 1.5 micron SiC layer as a coating on the monofilament surface. Test material No. 6 was a 2.5 micron BN layer as a coating on the monofilament surface.

Using the fiber coated with the sliding layer having a different thickness as described above, the core of the octagonal prism is alternately formed with three layers of 22.5 ° and 67.5 ° orientation angles. The preform was superimposed.

The obtained preform was impregnated with a matrix to produce a SiC-based composite material part.

[0097] A test piece was cut out from one piece of the octagonal composite material part thus obtained and subjected to a bending test. The bending test is a test in which a three-point bending load is applied to a test piece and the load and the deflection are measured.

After the preparation of the preform, the fiber of the outermost layer was cut off, and a yarn of 1 cm in length (monofilament 5
00) were observed with a scanning electron microscope to confirm the damage of the coating film. Table 2 shows the results.

As shown in Table 2, the test material No. 1 is that the density of the obtained composite material is 3.0 g / cm ³ , and the three-point bending strength at room temperature is σ1 of 210 MPa and σ2 of 420 MPa.
a, the breaking energy γ is 4.2 kj / m ² ,
Fracture showed a stable fracture behavior peculiar to the composite material, which did not occur until a complete fracture. Also, when checking the flaw detection status of the coating layer on the fiber surface after the preform production,
1.0%.

Test material No. No. 2, the density of the obtained composite material was 3.0 g / cm ³ , and the room temperature three-point bending strength was σ1.
Was 200 MPa, σ2 was 390 MPa, and the fracture energy γ was 4.0 kj / m ² , and the composite material exhibited stable fracture behavior unique to composite materials, which did not burst until complete fracture. Further, the state of flaw detection of the coating layer on the fiber surface after the preparation of the preform was 0.6%.

Sample No. In No. ³ , the density of the obtained composite material was 3.0 g / cm ³ , and the room temperature three-point bending strength was σ.
1 was 220 MPa, σ2 was 450 MPa, and the fracture energy γ was 4.6 kj / m ² , indicating a stable fracture behavior peculiar to the composite material, in which the fracture did not take place until complete fracture. Further, the state of flaw detection of the coating layer on the fiber surface after the preform was produced was 1.2%.

Sample No. No. 4, the density of the obtained composite material was 3.0 g / cm ³ , and the room temperature three-point bending strength was σ1.
Was 220 MPa, σ2 was 380 MPa, and the fracture energy γ was 4.2 kj / m ² , indicating that the composite material exhibited stable fracture behavior peculiar to the composite material, which did not reach a complete fracture until it was completely fractured. Further, the state of flaw detection of the coating layer on the fiber surface after preparation of the preform was 1.0%.

The test material N used for comparison was
o. 5, the density of the obtained composite material was 3.0 g / cm ³ ,
Regarding the three-point bending strength at room temperature, σ1 is 220 MPa, σ2
Is 280 MPa and the breaking energy γ is 1.5 kj /
m ^2, and after the highest intensity, it showed reduced drastically stress, then showed a fracture behavior indicating some composite properties. In addition, the flaw detection status of the coating layer on the fiber surface after the preparation of the preform was 15.0%.

Test material No. 6, the density of the obtained composite material was 3.0 g / cm ³ , and the room temperature three-point bending strength was σ1.
Was 220 MPa, σ2 was 240 MPa, and the fracture energy γ was 0.9 kj / m ^2. After exhibiting the highest strength, a monolithic fracture behavior showing a sharp decrease in stress was exhibited. Further, the state of flaw detection of the coating layer on the fiber surface after preparation of the preform was 25/0%.

Therefore, by defining the thickness of the sliding layer coated on the monofilament surface to be 0.1 to 2 μm, a stable fracture behavior peculiar to a composite material in which the failure does not occur at a stretch until complete failure is exhibited, It is possible to obtain a ceramic fiber composite material part having high properties.

Next, as a method of impregnating the matrix component into the preform, the effect of applying pressure will be described with reference to Table 3.

[0107]

[Table 3]

As shown in Table 3, the test material No. In 7,
When the matrix component was impregnated, the impregnation pressure was set to 15 MPa. In No. 8, the matrix component was impregnated in a normal pressure atmosphere without applying pressure.

Test material No. 7 and No. 7 8 has a 0.5 micron BN layer on the monofilament surface and 0.5
Fibers coated with a micron SiC layer were used.
These fibers were alternately stacked in three layers at an orientation angle of 22.5 degrees and 67.5 degrees and wound around an octagonal prism core to obtain a preform.

The obtained preform was impregnated with a matrix component to synthesize a SiC-based composite material, thereby obtaining a SiC-based composite material part. A bending test was performed using a test piece cut from one piece of the octagonal composite material part.

As shown in Table 3, the test material No. In 7,
The density of the obtained composite material is 3.0 g / cm ³ , and the room temperature three-point bending strength is σ1 of 220 Mfa and σ2 of 390 M.
Pa, the fracture energy γ was 4.0 kj / m ² , and the composite material exhibited a stable fracture behavior peculiar to the composite material, in which the fracture did not take place until complete fracture.

The test material No. 8
Then, the density of the obtained composite material was 2.9 g / cm ³ , and the three-point bending strength at room temperature was σ1 of 150 MPa and σ2 of 2
10 MPa and a breaking energy γ of 0.7 kj / m ²
And showed almost the same fracture behavior as the monolithic material. In addition, when the inside of the test piece was cut and observed inside, there were many regions rich in metal Si, and impregnation of the matrix component was insufficient. Was confirmed.

Therefore, when synthesizing the SiC matrix by the reaction sintering method, the impregnation of the matrix component at the time of molding is performed under pressure to further enhance the reliability of parts and the tolerance of damage, thereby improving the density of the ceramic fiber composite material. Parts can be manufactured.

[0114]

As described above, according to the ceramic fiber composite material part and the method of manufacturing the same according to the present invention, even in a high temperature range, the strength, the toughness and the oxidation resistance are excellent, and the manufacturing cost is reduced. Can be obtained.

[Brief description of the drawings]

FIG. 1 is a process chart schematically showing a manufacturing procedure in this embodiment.

FIG. 2 is a diagram showing a core used for producing a preform having a circular hole and obtaining a molded body in the embodiment.

3A and 3B are an external view showing an example of a fiber arrangement of a preform and a conceptual diagram for explaining a fiber orientation angle of a preform in the embodiment.

FIG. 4 is an external view (a) showing another example of the fiber arrangement of the preform and a conceptual diagram (b) for explaining the fiber orientation angle of the preform in the present embodiment.

5A and 5B are an external view showing another example of a fiber arrangement of a preform and a conceptual diagram for explaining a fiber orientation angle of a preform in the present embodiment.

FIG. 6 is a schematic diagram illustrating a matrix impregnation method using gas pressure in the present embodiment.

FIG. 7 is a schematic diagram showing a matrix impregnation method using hydraulic pressure in the present embodiment.

FIG. 8 is a schematic diagram showing an outer mold for limiting the amount of deposition when a matrix is impregnated in the embodiment.

[Explanation of symbols]

 Reference Signs List 1 core 1a impregnation core 1b winding core 2 pin 3 shaft 4 circular hole 5 67.5 degree oriented fiber 6 22.5 degree oriented fiber 7 75 degree oriented fiber 8 45 degree oriented fiber 9 15 degree oriented fiber 10 45-degree oriented fiber 11 Void 12 Closed container 13 Matrix slurry 14 Preform 15 Outer die 15a, 15b Outer die 15c Exhaust port 16 Vacuum pump 17 Compressor 18 Partition wall 19 Oil 20a, 20b Case body 21a, 22b Buffer material 22a, 22b Matrix Hole for slurry permeation

Claims (12)

[Claims] 1. A ceramic fiber composite material component obtained by compounding a ceramic matrix and a fiber, wherein a component wall has a hole by leaving a hole formed in a preform in a preform molding step of the fiber after the compound. A ceramic fiber composite material part characterized in that: 2. The ceramic fiber composite material part according to claim 1, wherein the composite fiber is a continuous fiber, and the composite after forming is a cylindrical member formed by laminating the continuous fibers at a plurality of orientation angles. Wherein the holes in the structural wall are:
A ceramic fiber composite material component, wherein the component is a gap formed in the laminated portion of the continuous fiber. 3. The ceramic fiber composite material component according to claim 1, wherein the orientation angles of the continuous fibers are θ1, θ2.
2... Θn, the axial stress component (Cos ²
The ratio between θ1 + Cos ² θ2 +... θn) and the circumferential stress component (Sin ² θ1 + Sin ² θ2 +. A ceramic fiber composite material part characterized in that: 4. The ceramic fiber composite material according to claim 1, wherein a silicon carbide ceramic formed by a reactive sintering method is applied as the ceramic matrix. Material parts. 5. The ceramic fiber composite material component according to claim 1, wherein the continuous fiber comprises a fiber main body containing silicon carbide as a main component and an interface layer covering the fiber main body. The interfacial layer is one or more coatings of at least one material selected from boron nitride, silicon carbide and carbon, and has a thickness of about 0.1 mm.
A ceramic fiber composite material part having a size of 1 to 2 microns. 6. A method of manufacturing a ceramic fiber composite material component for forming a composite of a ceramic matrix and fibers, wherein the fibers are laminated to form a preform having holes, and then the preform is impregnated with a ceramic matrix slurry. Ceramic matrix composite material characterized by producing a cylindrical body having a hole in a structural wall by drying and sintering the matrix slurry and integrating the matrix slurry with the preform. The method of manufacturing the part. 7. The preform according to claim 6, wherein continuous fibers are used as the composite fibers, and the continuous fibers are laminated at a plurality of orientation angles to form gaps between the fibers as holes. Forming a ceramic fiber composite material part. 8. The method for manufacturing a ceramic fiber composite material part according to claim 6, wherein the axial stress component (Cos ² θ1 + Cos ^{2) is} provided when the orientation angles of the continuous fibers are θ1, θ2,. θ2 +... θn) and a circumferential stress component (Sin ² θ1 + Sin ² θ2 +.
θn) is given by A method for producing a ceramic fiber composite material part. 9. The method for manufacturing a ceramic fiber composite material part according to claim 6, wherein a continuous fiber is formed by bundling a plurality of monofilaments into a fiber bundle as the composite fiber, and the continuous fiber forms a hole. To form a cylindrical preform having, after drying and degreasing the molded body,
A method for producing a ceramic fiber composite material part, characterized by obtaining a cylindrical part having a hole in a structural wall by firing by a reaction sintering method. 10. The method for producing a ceramic fiber composite material part according to claim 6, wherein the preform is inserted into a core made of a porous material, and in this state, the preform is inserted into a slurry container. A ceramic fiber composite material part characterized by being immersed in a matrix slurry of the core and reducing the pressure from an exhaust port arranged at the upper end portion of the slurry container of the core, so that the matrix slurry is deposited on the preform. Production method. 11. The method for producing a ceramic fiber composite material part according to claim 10, wherein the matrix slurry is supplied from outside the slurry container in a liquid pressure or a gas pressure of 0.1 to 3 times.
A method for producing a ceramic fiber composite material part, comprising applying pressure in a range of 0 MPa. 12. The method for producing a ceramic fiber composite material part according to claim 6, wherein, when the preform is impregnated with the matrix slurry, the outer surface of the preform in which the core has been fitted has a shape similar to that of the preform. A method of manufacturing a ceramic fiber composite material part, wherein the wall part is covered by a case body having a through hole for matrix slurry permeation.