WO2016002914A1 - Tubular body - Google Patents

Tubular body Download PDF

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Publication number
WO2016002914A1
WO2016002914A1 PCT/JP2015/069214 JP2015069214W WO2016002914A1 WO 2016002914 A1 WO2016002914 A1 WO 2016002914A1 JP 2015069214 W JP2015069214 W JP 2015069214W WO 2016002914 A1 WO2016002914 A1 WO 2016002914A1
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WO
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Prior art keywords
sic
tubular body
fiber
layer
ceramic
Prior art date
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PCT/JP2015/069214
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French (fr)
Japanese (ja)
Inventor
久保　修一
高木　俊
Original Assignee
イビデン株式会社
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Publication date
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Publication of WO2016002914A1 publication Critical patent/WO2016002914A1/en

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
    • G21C3/30—Assemblies of a number of fuel elements in the form of a rigid unit
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21C—NUCLEAR REACTORS
    • G21C3/00—Reactor fuel elements and their assemblies; Selection of substances for use as reactor fuel elements
    • G21C3/30—Assemblies of a number of fuel elements in the form of a rigid unit
    • G21C3/32—Bundles of parallel pin-, rod-, or tube-shaped fuel elements
    • G21C3/324—Coats or envelopes for the bundles
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Definitions

  • the present invention relates to a polygonal tubular body made of a ceramic / ceramic composite material and a SiC / SiC composite material.
  • a tubular body made of a SiC / SiC composite material has high-strength SiC fibers as an aggregate, and SiC mainly forms a matrix. Since SiC is a material having heat resistance and oxidation resistance, it has a feature that it can be used in an oxidizing atmosphere in which a C / C composite (carbon fiber reinforced carbon composite material) cannot be used.
  • a SiC layer is formed on at least the outer surface of a tubular fiber-reinforced carbonaceous substrate made of an aggregate made of ceramic fibers and a carbonaceous material filled between the ceramic fibers, and the fiber-reinforced carbonaceous material
  • a tubular body is described in which silicon atoms are diffused from the boundary region between the substrate and the SiC layer toward the inside of the fiber-reinforced carbonaceous substrate.
  • the process can be simplified, and the reactor can be operated at a higher temperature by improving performance, so that an energy efficient nuclear reactor can be provided. It is described that the service life can be extended.
  • the tubular body made of the SiC / SiC composite described above has only a description regarding a cylindrical shape, and there is no description regarding a polygonal tubular body such as a quadrangle.
  • An object of the present invention is to provide a tubular body that can solve various problems that may occur in the case of a tubular body of a polygonal SiC / SiC composite such as a quadrangle.
  • a tubular body of the present invention for solving the above-mentioned problems is provided with a plurality of ceramic fiber layers, a fiber coating layer covering the plurality of ceramic fiber layers, and a gap between the ceramic fiber layers and an outer surface.
  • the ceramic fiber layer has a smaller winding angle with respect to the axis of the mandrel than the ceramic fiber layer immediately below the outermost ceramic fiber layer.
  • the tubular body of the present invention for solving the above-mentioned problems is provided with a plurality of SiC fiber layers, a fiber coating layer covering the plurality of SiC fiber layers, and a gap between the SiC fiber layers and an outer surface.
  • a polygonal tubular body made of a SiC / SiC composite material comprising a CVD-SiC layer to be formed, the longitudinal side of the tubular body having an R-plane, and the SiC fiber layer being an outermost layer
  • the SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
  • the tubular body of the present invention has a plurality of ceramic fiber layers or SiC fiber layers having different winding angles with respect to the mandrel axis. For this reason, it arrange
  • the plurality of ceramic fiber layers or SiC fiber layers are filled with CVD-SiC in the gaps, so that the fibers can be strongly connected. For this reason, a high strength tubular body can be obtained. Further, since the longitudinal side of the tubular body has an R surface, the ceramic fiber or the SiC fiber bends gently, and the tension applied to the fiber surface on the extending side can be reduced. Further, the ceramic fiber layer or SiC fiber layer has an outermost ceramic fiber layer or SiC fiber layer winding angle with respect to the mandrel axis more than the ceramic fiber layer or SiC fiber layer immediately below the outermost ceramic fiber layer or SiC fiber layer. Is small.
  • the tubular body of the present invention is desirably in the following manner.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 to 60 degrees.
  • the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 degrees or more, the outermost ceramic fiber layer or SiC fiber layer is firmly wound around the tubular body. Therefore, a tubular body in which the ceramic fiber layer or the SiC fiber layer is difficult to peel can be formed.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the mandrel axis is 60 degrees or less, the radius of curvature of the bending of the ceramic fiber or SiC fiber bent along the longitudinal side of the mandrel is increased. The effect is exhibited, the stress accompanying the strain can be relaxed, and a strong tubular body can be obtained.
  • the tubular body has a quadrangular cross section.
  • a plurality of tubular bodies can be regularly arranged, and various things can be stored inside the tubular body, so that the space can be used effectively.
  • the radius of curvature of the R surface is 5 to 20 mm.
  • the radius of curvature of the R plane is 5 mm or more, the stress applied to the ceramic fiber or SiC fiber bent along the R plane can be relaxed.
  • the radius of curvature of the R surface is 20 mm or less, it is possible to reduce the space that cannot be used by the R surface.
  • the ceramic fiber layer or the SiC fiber layer is composed of ceramic fibers having a fiber diameter of 5 to 20 ⁇ m.
  • the fiber diameter of the ceramic fiber is 5 ⁇ m or more, the influence of defects such as minute scratches generated on the fiber surface can be reduced, and the ceramic fiber can be made difficult to break.
  • the fiber diameter of the ceramic fiber is 20 ⁇ m or less, the tension generated on the outer surface on the side extending along with the bending can be suppressed, and it is possible to obtain a strong tubular body that can be hardly broken.
  • the fiber coating layer contains one or more elements selected from metal elements, silicon, carbon, and boron.
  • the tubular body is for nuclear power.
  • the tubular body of the present invention is made of a ceramic / ceramic composite material or a SiC / SiC composite material, has heat resistance, and has high strength, so that it can be used for nuclear power such as a channel box for storing nuclear fuel. Can be suitably used.
  • the tubular body of the present invention has a plurality of ceramic fiber layers or SiC fiber layers having different winding angles with respect to the mandrel axis. For this reason, it arrange
  • the plurality of ceramic fiber layers or SiC fiber layers are filled with CVD-SiC in the gaps, so that the fibers can be strongly connected. For this reason, a high strength tubular body can be obtained. Further, since the longitudinal side of the tubular body has an R surface, the ceramic fiber or the SiC fiber bends gently, and the tension applied to the fiber surface on the extending side can be reduced. Further, the ceramic fiber layer or the SiC fiber layer is wound around the mandrel axis more than the ceramic fiber layer or the SiC fiber layer of the outermost layer directly under the outermost layer of the ceramic fiber layer or directly under the outermost SiC fiber layer. The angle is small. For this reason, the matrix formed by CVD with few fiber fluffs can obtain the tubular body which consists of SiC / SiC composite material with few adhesion to the fluffed SiC fiber, and few pinholes.
  • Process flow figure of manufacturing method of tubular body of Embodiment 1 of the present invention The perspective view of the mandrel used for manufacture of Embodiment 1 of this invention
  • the detailed process flow figure of the winding process of the tubular body of Embodiment 1 of this invention Drawing showing the appearance photograph of the tubular body of Embodiment 1 of the present invention Sectional drawing of the tubular body of Embodiment 1 of this invention
  • This specification mainly describes a SiC / SiC composite material composed of a SiC fiber and a CVD-SiC matrix.
  • the present invention is also effective for a ceramic / ceramic composite material composed of a ceramic fiber and a ceramic-CVD matrix.
  • the SiC fiber corresponds to the ceramic fiber
  • the CVD-SiC corresponds to the ceramic-CVD and can be described by being replaced.
  • Examples of CVD-SiC include SiC, titanium silicon carbide, alumina, TaC, TaN, and SiO 2 . Further, the combination of ceramic fiber and ceramic-CVD is not particularly limited.
  • the axis of the mandrel is the central axis in the longitudinal direction of the mandrel.
  • the winding angle with respect to the axis of the mandrel is an angle at which the SiC fiber intersects with a line parallel to the axis of the mandrel. In the case of 0 degrees, the SiC fiber is wound in the longitudinal direction of the mandrel, and in the case of 90 degrees, the SiC fiber is wound around the mandrel.
  • tubular body of the present invention will be described.
  • the tubular body of the present invention includes a plurality of ceramic fiber layers, a fiber coating layer that covers the plurality of ceramic fiber layers, a CVD-ceramic layer that fills a gap between the ceramic fiber layers and forms an outer surface.
  • the tubular body of the present invention includes a plurality of SiC fiber layers, a fiber coating layer that covers the plurality of SiC fiber layers, a CVD-SiC layer that fills a gap between the SiC fiber layers and constitutes an outer surface.
  • the tubular body of the present invention has a plurality of ceramic fiber layers or SiC fiber layers having different winding angles with respect to the mandrel axis. For this reason, it arrange
  • the plurality of ceramic fiber layers or SiC fiber layers are filled with CVD-SiC in the gaps, so that the fibers can be strongly connected. For this reason, a high strength tubular body can be obtained. Further, since the side in the longitudinal direction of the tubular body has an R surface, the ceramic fiber layer or the SiC fiber bends gently, and the tension applied to the fiber surface on the extending side can be reduced. Further, the ceramic fiber layer or SiC fiber layer has an outermost ceramic fiber layer or SiC fiber layer winding angle with respect to the mandrel axis more than the ceramic fiber layer or SiC fiber layer immediately below the outermost ceramic fiber layer or SiC fiber layer. Is small. For this reason, the matrix formed by CVD with few fiber fluffing can obtain the tubular body which consists of a SiC / SiC composite material with few pinholes with few adhesion to the fluffed ceramic fiber layer or SiC fiber.
  • the tubular body of the present invention is desirably in the following manner.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 to 60 degrees.
  • the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 degrees or more, the outermost ceramic fiber layer or SiC fiber layer is firmly wound around the tubular body. Therefore, a tubular body in which the ceramic fiber layer or the SiC fiber layer is difficult to peel can be formed.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the mandrel axis is 60 degrees or less, the radius of curvature of the bending of the ceramic fiber or SiC fiber bent along the longitudinal side of the mandrel is increased. The effect is exhibited, the stress accompanying the strain can be relaxed, and a strong tubular body can be obtained.
  • the tubular body has a quadrangular cross section.
  • a plurality of tubular bodies can be regularly arranged, and various things can be stored inside the tubular body, so that the space can be used effectively.
  • the radius of curvature of the R surface is 5 to 20 mm.
  • the radius of curvature of the R plane is 5 mm or more, the stress applied to the ceramic fiber or SiC fiber bent along the R plane can be relaxed.
  • the radius of curvature of the R surface is 20 mm or less, it is possible to reduce the space that cannot be used by the R surface.
  • the ceramic fiber layer or the SiC fiber layer is composed of ceramic fibers having a fiber diameter of 5 to 20 ⁇ m.
  • the fiber diameter of the ceramic fiber is 5 ⁇ m or more, the influence of defects such as minute scratches generated on the fiber surface can be reduced, and the ceramic fiber can be made difficult to break.
  • the fiber diameter of the ceramic fiber is 20 ⁇ m or less, the tension generated on the outer surface on the side extending along with the bending can be suppressed, and it is possible to obtain a strong tubular body that can be hardly broken.
  • the fiber coating layer contains one or more elements selected from metal elements, silicon, carbon, and boron.
  • the tubular body is for nuclear power.
  • the tubular body of the present invention is made of a ceramic / ceramic composite material or a SiC / SiC composite material, has heat resistance, and has high strength, so that it can be used for nuclear power such as a channel box for storing nuclear fuel. Can be suitably used.
  • SiC fibers are wound around a polygonal mandrel having an R-shaped portion on the longitudinal side, and a plurality of SiC fiber layers having different winding angles with respect to the axis of the mandrel are laminated.
  • a winding process for obtaining a wound body a CVD process for coating the wound body with SiC-CVD and forming a covering body, and a mandrel removing process for removing the mandrel from the covering body,
  • Each SiC fiber layer is characterized in that the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
  • SiC fiber is a high strength and high elasticity fiber, it exhibits a high strength against tension, but has a large amount of stress generated against strain and is easy to break. For this reason, in a polygonal tubular body that requires sharp bending, fibers are broken at the corner portion, and fluffing is likely to occur. In this invention, since it has R surface in the side of the longitudinal direction of a mandrel, the stress accompanying the bending of a SiC fiber can be made small and it cannot be broken easily.
  • the curvature radius of the bending of the SiC fiber can be further increased and the stress accompanying the bending can be reduced. Furthermore, by arranging the SiC fiber layer having a small winding angle with respect to the axis of the mandrel in the outermost layer, it can be more difficult to break than the SiC fiber layer immediately below the outermost SiC fiber layer. That is, it is possible to cover the SiC fiber layer that is easily fluffed with the SiC fiber layer that is difficult to fluff, and to suppress the occurrence of fluff.
  • the tubular body of the present invention has a plurality of SiC fiber layers having different winding angles with respect to the axis of the mandrel. For this reason, it arrange
  • the fibers can be strongly connected.
  • the tubular body of the present invention is manufactured as follows. (1) Between the winding step and the CVD step, the method further includes a coating step of baking after applying a coating material to the wound body. Since the CVD process is exposed to a high temperature, the SiC fiber is burdened by the difference in thermal expansion, and is likely to cause fluffing. In the present invention, since a fiber coating layer is formed on the SiC fiber by adding a coating process before the CVD process in which SiC fiber is likely to fluff, and the SiC fibers are bound to each other, the occurrence of fluff can be suppressed. it can.
  • CVD-SiC is deposited on the fuzz and the source gas does not spread sufficiently inside the wound body, making it easy to make defects such as pinholes in the tubular body, With such a configuration, the CVD-SiC is uniformly coated, and generation of defects due to fluffing can be suppressed.
  • a fiber coating layer is formed on the surface of the SiC fiber by a coating process. Since the fiber coating layer is formed at the interface between the CVD-SiC matrix and the SiC fiber, the stress can be dispersed so that cracks extending from the matrix are not transmitted to the SiC fiber. By these actions, a tubular body made of a high-strength SiC / SiC composite material can be obtained.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 to 60 degrees.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 degrees or more, the outermost ceramic fiber layer or SiC fiber layer is firmly wound around the tubular body. A tubular body that is difficult to peel can be formed.
  • the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 60 degrees or less, the radius of curvature of the bending of the ceramic fiber or SiC fiber bent along the longitudinal side of the mandrel is increased. And stress associated with strain can be relaxed.
  • the tubular body has a quadrangular cross section.
  • a plurality of tubular bodies can be regularly arranged, and various things can be stored inside the tubular body, so that the space can be used effectively.
  • the radius of curvature of the R-surface shaped part is 5 to 20 mm.
  • the radius of curvature of the R-plane shape portion is 5 mm or more, the stress applied to the SiC fiber that is bent along the R-plane can be relaxed.
  • the radius of curvature of the R-surface shape portion is 20 mm or less, it is possible to reduce an unusable space that can be generated by the R-surface shape portion.
  • the ceramic fiber layer or the SiC fiber layer is composed of ceramic fibers having a fiber diameter of 5 to 20 ⁇ m.
  • the fiber diameter of the ceramic fiber is 5 ⁇ m or more, the influence of defects such as minute scratches generated on the fiber surface can be reduced, and the ceramic fiber can be made difficult to break.
  • the fiber diameter of the ceramic fiber is 20 ⁇ m or less, it is possible to suppress the tension generated on the outer surface on the side extending along with the bending and make it difficult to break.
  • the coating material is a compound containing one or more elements selected from metal elements, silicon, carbon, and boron. These compounds remain on the surface of the SiC fiber by firing to form a fiber coating layer. Since the fiber coating layer is interposed at the interface between the CVD-SiC matrix and the SiC fibers, it has an action of suppressing the extension of cracks from the matrix.
  • the tubular body is for nuclear power.
  • the tubular body of the present invention is composed of a SiC / SiC composite material, has heat resistance, and has high strength, so that it can be suitably used for nuclear power such as a channel box for storing nuclear fuel. Can do.
  • Embodiment 1 of the manufacturing method of the tubular body of this invention is demonstrated.
  • the manufacturing method of the tubular body of Embodiment 1 includes a winding process (FIG. 1A), a coating process (FIG. 1B), a CVD process (FIG. 1C), and a mandrel removing process (FIG. 1D). )).
  • the mandrel used in the production of the tubular body of the present invention is not particularly limited as long as it has heat resistance because it is fired and CVD-treated while the SiC fiber is wound.
  • graphite, SiC, etc. can be used.
  • an isotropic graphite material or the like can be used.
  • An isotropic graphite material has a thermal expansion coefficient close to that of SiC, so that thermal distortion is unlikely to occur during heating and cooling. Further, there is an advantage that graphite can be removed by air oxidation in a later mandrel removal step.
  • the graphite mandrel 1 While the graphite mandrel 1 is rotated, it is wound in the form of a strand in which a plurality of SiC fibers are bundled.
  • the SiC fiber is not particularly limited.
  • Ube Industries, Ltd. SiC fiber "Tyranno SA" can be used.
  • the fiber diameter is 7.5 ⁇ m.
  • the graphite mandrel 1 is a square having a side length of 130 mm in cross section, and an R-plane shape portion 2 having a 10 mm corner portion.
  • the length of the graphite mandrel 1 is 1000 mm.
  • FIG. 2 shows a perspective view of the mandrel.
  • the four sides in the longitudinal direction of the mandrel 1 have R-shaped portions.
  • FIG. 3A showing the first layer
  • the SiC fiber is wound while being alternately moved so as to be 45 degrees with respect to the axis of the mandrel. Since it winds while moving alternately, it becomes a helical winding in which a rhombus pattern is formed on the surface.
  • FIG.3 (b) which shows the 2nd layer, it winds with the form of the strand which bundled several SiC fiber so that it might become 0 degree
  • FIG.3 (c) which shows the 3rd layer
  • Such a winding method is hoop winding.
  • FIG. 3D showing the fourth layer the SiC fiber is wound while being alternately moved so as to be 45 degrees with respect to the axis of the mandrel. Since it winds while moving alternately, it becomes a helical winding in which a rhombus pattern is formed on the surface. In this way, a wound body having four SiC fiber layers is obtained.
  • the fourth SiC fiber layer that is the outermost layer has a winding angle of 45 degrees with respect to the axis of the mandrel, and the third SiC fiber layer immediately below the outermost SiC fiber layer is 90 degrees with respect to the axis of the mandrel. It is a winding angle.
  • a wound body is obtained in which the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer. Since the SiC fiber is wound around the mandrel having the R-shaped portion 2 on the long side, it is possible to make it difficult to apply a large bending stress to the SiC fiber.
  • the SiC fiber is wound so that the third-layer SiC fiber is orthogonal to the axis of the mandrel, the SiC fiber is wound with a curvature radius equivalent to the curvature radius of the R-surface shape portion of the mandrel.
  • the mandrel of the fourth outermost layer is wound at an angle of 45 degrees with respect to the axis of the mandrel, so the radius of curvature of the actually wound SiC fiber is (1 / cos 45 degrees), that is, It is relaxed 1.41 times and can be made more difficult to break.
  • the coating material is a compound containing one or more elements selected from metal elements, silicon, carbon, and boron.
  • the coating material is a phenol resin, and a fiber coating layer is formed on the surface of the SiC fiber by firing. These compounds remain on the surface of the SiC fiber by firing to form a fiber coating layer. Since the fiber coating layer is interposed at the interface between the CVD-SiC matrix and the SiC fibers, it has an action of suppressing the extension of cracks from the matrix.
  • the coating process is not essential, but it is desirable to use the method for manufacturing a tubular body because it has the effect of making the SiC / SiC composite material difficult to break.
  • coating materials include organic substances such as polycarbosilane, polyorganoboronsilazane, furan resin, organometallic compounds, and ceramic fine particles such as nano silica.
  • Firing can be performed at 400 to 1000 ° C., for example.
  • the firing atmosphere can be appropriately selected depending on the form of the fiber coating layer to be formed. For example, in the case of a carbon-based fiber coating layer, a reducing atmosphere is used, and in the case of an oxide-based fiber coating layer, an oxidizing atmosphere is used. Thus, a desired fiber coating layer can be obtained.
  • FIG. 1 (c) The wound body thus obtained is placed in a CVD furnace and covered with CVD-SiC.
  • the film forming temperature can be 1000 to 1800 ° C., for example.
  • the source gas is not particularly limited.
  • a mixed gas of silane gas / methane gas, a mixed gas of tetrachlorosilane gas / methane gas, methyltrichlorosilane (MTS), or the like can be used.
  • hydrogen gas or the like for adjusting the partial pressure in the furnace can be used as appropriate.
  • the type of CVD is not particularly limited, but it can be used in either a hot wall type that heats the entire furnace by radiation of the heater in the furnace, or a cold wall type that heats only the wound body by a heater built into the mandrel. it can.
  • a hot wall type that heats the entire furnace by radiation of the heater in the furnace
  • a cold wall type that heats only the wound body by a heater built into the mandrel. it can.
  • CVD-SiC not only fills the space between the SiC fibers but also deposits it to have a surface layer made of only CVD-SiC.
  • FIG. 1 (d) By removing the mandrel thus obtained, a tubular body made of a square SiC / SiC composite material can be obtained.
  • the method for removing the mandrel is not particularly limited. Any method can be used, such as a cutting method that is mechanically cut and removed, a combustion method that burns in an oxidizing atmosphere furnace, or a pulling method that is pulled out by an external force such as hydraulic pressure, and these methods may be used in combination. Furthermore, the both ends of the tubular body are cut to adjust the shape.
  • FIG. 4 is a drawing showing an external appearance photograph of the tubular body obtained by the manufacturing method of the first embodiment. It has a diamond-shaped pattern on the surface that is characteristic of helical winding.
  • FIGS. 5A to 5C are cross-sectional views of the tubular body of the first embodiment. It has a SiC fiber layer 4 and a matrix 5 made of CVD-SiC. The matrix 5 made of CVD-SiC not only fills between the fibers, but further deposits and has a surface layer portion made only of CVD-SiC.
  • the tubular body 10 thus obtained has a plurality of SiC fiber layers 4, a fiber coating layer 8 that covers the plurality of SiC fiber layers 4, and a gap between the SiC fiber layers 4 and an outer surface.
  • the SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
  • the tubular body 10 of Embodiment 1 has a plurality of SiC fiber layers 4 having different winding angles with respect to the mandrel axis. For this reason, it arrange
  • the gaps are filled with CVD-SiC 5, so that the fibers can be strongly connected. For this reason, the high strength tubular body 10 can be obtained. Further, since the side in the longitudinal direction of the tubular body 10 has the R surface 6, the SiC fiber bends gently, and the tension applied to the extending fiber surface can be reduced.
  • the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer. For this reason, the matrix formed by CVD with few fiber fluffs can obtain the tubular body which consists of SiC / SiC composite material with few adhesion to the fluffed SiC fiber, and few pinholes.

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Abstract

This invention provides a tubular body that makes it possible to solve a variety of problems that can occur when using a tubular body consisting of a tetragonal or otherwise polygonal ceramic/ceramic or SiC/SiC composite material. The provided tubular body is a polygonal tubular body (10) comprising a SiC/SiC composite material that comprises the following: a plurality of SiC fiber layers (4); a fiber-coating layer (8) that coats said SiC fiber layers (4); and a CVD SiC layer that fills gaps between the SiC fiber layers (4) and constitutes the outer surface of the SiC/SiC composite material. The lengthwise edges of said tubular body (10) have rounded surfaces (6), and the winding angle of the outermost SiC fiber layer with respect to a mandrel axis is smaller than that of the SiC fiber layer immediately beneath said outermost SiC fiber layer.

Description

管状体Tubular body
　本発明は、セラミック／セラミック複合材及びＳｉＣ／ＳｉＣ複合材からなる多角形の管状体に関する。 The present invention relates to a polygonal tubular body made of a ceramic / ceramic composite material and a SiC / SiC composite material.
　ＳｉＣ／ＳｉＣ複合材からなる管状体は、高強度のＳｉＣ繊維を骨材とし、主にＳｉＣがマトリックスを構成する。ＳｉＣは、耐熱性を有するとともに耐酸化性のある素材であるので、Ｃ／Ｃコンポジット（炭素繊維強化炭素複合材）が使用できない酸化雰囲気下で使用できる特徴がある。 A tubular body made of a SiC / SiC composite material has high-strength SiC fibers as an aggregate, and SiC mainly forms a matrix. Since SiC is a material having heat resistance and oxidation resistance, it has a feature that it can be used in an oxidizing atmosphere in which a C / C composite (carbon fiber reinforced carbon composite material) cannot be used.
　特許文献１には、セラミック繊維からなる骨材と前記セラミック繊維間に充填された炭素質とからなる管状の繊維強化炭素質基材の少なくとも外表面にＳｉＣ層が形成され、前記繊維強化炭素質基材と前記ＳｉＣ層の境界領域から当該繊維強化炭素質基材の内部に向かってケイ素原子が拡散してなる管状体が記載されている。
　このような管状体では、セラミック繊維の表面が、炭素質に接しているため、熱応力により発生するクラックを、セラミック繊維表面で止めることができ、管状体の内外を貫通するクラックが発生しにくい上、個々のセラミック繊維に被覆を設ける前処理が必要ないため工程が簡略化でき、性能向上によりさらには原子炉をより高温で運転できるため、エネルギー効率の高い原子炉を提供することができると共に使用寿命が長期化可能であることが記載されている。 In Patent Document 1, a SiC layer is formed on at least the outer surface of a tubular fiber-reinforced carbonaceous substrate made of an aggregate made of ceramic fibers and a carbonaceous material filled between the ceramic fibers, and the fiber-reinforced carbonaceous material A tubular body is described in which silicon atoms are diffused from the boundary region between the substrate and the SiC layer toward the inside of the fiber-reinforced carbonaceous substrate.
In such a tubular body, since the surface of the ceramic fiber is in contact with the carbonaceous material, cracks caused by thermal stress can be stopped at the surface of the ceramic fiber, and cracks penetrating the inside and outside of the tubular body are unlikely to occur. In addition, since no pretreatment is required to provide coatings on individual ceramic fibers, the process can be simplified, and the reactor can be operated at a higher temperature by improving performance, so that an energy efficient nuclear reactor can be provided. It is described that the service life can be extended.
日本国特開２００９－２１０２６６号公報Japanese Unexamined Patent Publication No. 2009-210266
　しかしながら、前記記載のＳｉＣ／ＳｉＣ複合材よりなる管状体は、円筒形の形状に関する記載があるのみで、四角形など多角形の管状体に関しては何の記載もない。
　実際多角形の管状体を製造する際には、円筒形状の管状体には無い課題がある。本発明では、四角形など多角形のＳｉＣ／ＳｉＣ複合材の管状体の場合におこりうる様々な問題を解決可能な管状体を提供することを目的とする。 However, the tubular body made of the SiC / SiC composite described above has only a description regarding a cylindrical shape, and there is no description regarding a polygonal tubular body such as a quadrangle.
When actually manufacturing a polygonal tubular body, there is a problem that is not found in a cylindrical tubular body. An object of the present invention is to provide a tubular body that can solve various problems that may occur in the case of a tubular body of a polygonal SiC / SiC composite such as a quadrangle.
　前記課題を解決するための本発明の管状体は、複数層のセラミック繊維層と、前記複数層のセラミック繊維層を被覆する繊維被覆層と、前記セラミック繊維層の隙間を充填するとともに外表面を構成するＣＶＤ－セラミック層とからなるセラミック／セラミック複合材からなる多角形の管状体であって、前記管状体の長手方向の辺は、Ｒ面を有し、前記セラミック繊維層は、最外層のセラミック繊維層が、前記最外層セラミック繊維層直下のセラミック繊維層よりもマンドレルの軸線に対する巻き角度が小さい。 A tubular body of the present invention for solving the above-mentioned problems is provided with a plurality of ceramic fiber layers, a fiber coating layer covering the plurality of ceramic fiber layers, and a gap between the ceramic fiber layers and an outer surface. A polygonal tubular body made of a ceramic / ceramic composite material comprising a CVD-ceramic layer to be formed, the longitudinal side of the tubular body having an R surface, and the ceramic fiber layer being an outermost layer The ceramic fiber layer has a smaller winding angle with respect to the axis of the mandrel than the ceramic fiber layer immediately below the outermost ceramic fiber layer.
　前記課題を解決するための本発明の管状体は、複数層のＳｉＣ繊維層と、前記複数層のＳｉＣ繊維層を被覆する繊維被覆層と、前記ＳｉＣ繊維層の隙間を充填するとともに外表面を構成するＣＶＤ－ＳｉＣ層とからなるＳｉＣ／ＳｉＣ複合材からなる多角形の管状体であって、前記管状体の長手方向の辺は、Ｒ面を有し、前記ＳｉＣ繊維層は、最外層のＳｉＣ繊維層が、前記最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。 The tubular body of the present invention for solving the above-mentioned problems is provided with a plurality of SiC fiber layers, a fiber coating layer covering the plurality of SiC fiber layers, and a gap between the SiC fiber layers and an outer surface. A polygonal tubular body made of a SiC / SiC composite material comprising a CVD-SiC layer to be formed, the longitudinal side of the tubular body having an R-plane, and the SiC fiber layer being an outermost layer The SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
　本発明の管状体によれば、マンドレルの軸線に対する巻き角度が異なる複数層のセラミック繊維層あるいはＳｉＣ繊維層を有している。このため、管状体にかかる様々な方向の力に対し、いずれかのセラミック繊維層あるいはＳｉＣ繊維層に張力がかかるように配置される。このため、高強度の管状体を得ることができる。 The tubular body of the present invention has a plurality of ceramic fiber layers or SiC fiber layers having different winding angles with respect to the mandrel axis. For this reason, it arrange | positions so that tension | tensile_strength may be applied to any ceramic fiber layer or SiC fiber layer with respect to the force of the various directions concerning a tubular body. For this reason, a high intensity | strength tubular body can be obtained.
　本発明の管状体によれば、複数層のセラミック繊維層あるいはＳｉＣ繊維層は、隙間をＣＶＤ－ＳｉＣによって充填されるので、繊維どうしを強く結びつけることができる。このため高強度の管状体を得ることができる。
　また、管状体の長手方向の辺は、Ｒ面を有しているので、セラミック繊維あるいはＳｉＣ繊維が緩やかに曲がり、延びる側の繊維表面にかかる張力を小さくすることができる。さらにセラミック繊維層あるいはＳｉＣ繊維層は、最外層のセラミック繊維層あるいはＳｉＣ繊維層が、最外層セラミック繊維層あるいは最外層ＳｉＣ繊維層直下のセラミック繊維層あるいはＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。このため、繊維の毛羽立ちが少なく、ＣＶＤによって形成されるマトリックスは、毛羽立ちしたセラミック繊維あるいはＳｉＣ繊維への付着が少なく、ピンホールの少ないＳｉＣ／ＳｉＣ複合材よりなる管状体を得ることができる。 According to the tubular body of the present invention, the plurality of ceramic fiber layers or SiC fiber layers are filled with CVD-SiC in the gaps, so that the fibers can be strongly connected. For this reason, a high strength tubular body can be obtained.
Further, since the longitudinal side of the tubular body has an R surface, the ceramic fiber or the SiC fiber bends gently, and the tension applied to the fiber surface on the extending side can be reduced. Further, the ceramic fiber layer or SiC fiber layer has an outermost ceramic fiber layer or SiC fiber layer winding angle with respect to the mandrel axis more than the ceramic fiber layer or SiC fiber layer immediately below the outermost ceramic fiber layer or SiC fiber layer. Is small. For this reason, it is possible to obtain a tubular body made of a SiC / SiC composite material with less fluffing of fibers, a matrix formed by CVD having less adhesion to fuzzy ceramic fibers or SiC fibers, and few pinholes.
　本発明の管状体は、以下の態様であることが望ましい。
（１）前記最外層のセラミック繊維層またはＳｉＣ繊維層は、前記マンドレルの軸線に対する巻き角度が３０～６０度である。
　本発明の管状体は、最外層のセラミック繊維層あるいはＳｉＣ繊維層のマンドレルの軸線に対する巻き角度が、３０度以上であると、最外層のセラミック繊維層あるいはＳｉＣ繊維層が管状体に強固に巻き付けられるので、セラミック繊維層あるいはＳｉＣ繊維層の剥離しにくい管状体を構成することができる。最外層のセラミック繊維層あるいはＳｉＣ繊維層のマンドレルの軸線に対する巻き角度が、６０度以下であると、マンドレルの長手方向の辺に沿って曲げられるセラミック繊維あるいはＳｉＣ繊維の曲げの曲率半径を大きくする効果が発揮され、歪みに伴う応力を緩和することができ強固な管状体を得ることができる。 The tubular body of the present invention is desirably in the following manner.
(1) The winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 to 60 degrees.
In the tubular body of the present invention, when the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 degrees or more, the outermost ceramic fiber layer or SiC fiber layer is firmly wound around the tubular body. Therefore, a tubular body in which the ceramic fiber layer or the SiC fiber layer is difficult to peel can be formed. When the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the mandrel axis is 60 degrees or less, the radius of curvature of the bending of the ceramic fiber or SiC fiber bent along the longitudinal side of the mandrel is increased. The effect is exhibited, the stress accompanying the strain can be relaxed, and a strong tubular body can be obtained.
（２）前記管状体は、断面が四角形である。
　四角形の管状体は、複数の管状体を規則的に配列することができ、かつ、管状体の内部に様々なものを収納することができ空間を有効に利用することができる。 (2) The tubular body has a quadrangular cross section.
In the rectangular tubular body, a plurality of tubular bodies can be regularly arranged, and various things can be stored inside the tubular body, so that the space can be used effectively.
（３）前記Ｒ面の曲率半径は、５～２０ｍｍである。
　Ｒ面の曲率半径が、５ｍｍ以上であると、Ｒ面に沿って曲がるセラミック繊維あるいはＳｉＣ繊維にかかる応力を緩和することができる。Ｒ面の曲率半径が、２０ｍｍ以下であると、Ｒ面によってできる利用できない空間を少なくすることができる。 (3) The radius of curvature of the R surface is 5 to 20 mm.
When the radius of curvature of the R plane is 5 mm or more, the stress applied to the ceramic fiber or SiC fiber bent along the R plane can be relaxed. When the radius of curvature of the R surface is 20 mm or less, it is possible to reduce the space that cannot be used by the R surface.
（４）前記セラミック繊維層または前記ＳｉＣ繊維層は、繊維直径が５～２０μｍのセラミック繊維で構成される。
　セラミック繊維の繊維直径が５μｍ以上であると繊維表面に発生する微少な傷などの欠陥の影響を小さくすることができ、折れにくくすることができる。セラミック繊維の繊維直径が２０μｍ以下であると、曲げに伴って延びる側の外表面に発生する張力を抑制することができ、折れにくくすることができ強固な管状体を得ることができる。 (4) The ceramic fiber layer or the SiC fiber layer is composed of ceramic fibers having a fiber diameter of 5 to 20 μm.
When the fiber diameter of the ceramic fiber is 5 μm or more, the influence of defects such as minute scratches generated on the fiber surface can be reduced, and the ceramic fiber can be made difficult to break. When the fiber diameter of the ceramic fiber is 20 μm or less, the tension generated on the outer surface on the side extending along with the bending can be suppressed, and it is possible to obtain a strong tubular body that can be hardly broken.
（５）前記繊維被覆層は、金属元素、シリコン、炭素、ホウ素から選択される１または２以上の元素を含有する。
　これらの元素からなる繊維被覆層がＳｉＣ繊維の表面に有することによって、セラミック繊維あるいはＳｉＣ繊維とマトリックスとの界面に異質な物質を介在させることができる。繊維被覆層が、ＣＶＤ－ＳｉＣからなるマトリックスとセラミック繊維あるいはＳｉＣ繊維との界面に介在することにより、マトリックスからのクラックの伸展を抑制する作用がある。 (5) The fiber coating layer contains one or more elements selected from metal elements, silicon, carbon, and boron.
By having the fiber coating layer made of these elements on the surface of the SiC fiber, a foreign substance can be interposed at the interface between the ceramic fiber or the SiC fiber and the matrix. When the fiber coating layer is interposed at the interface between the CVD-SiC matrix and the ceramic fiber or SiC fiber, there is an action of suppressing the extension of cracks from the matrix.
（６）前記管状体は、原子力用である。
　本発明の管状体は、セラミック／セラミック複合材あるいはＳｉＣ／ＳｉＣ複合材で構成され、耐熱性を有している上に、高い強度を備えているので、原子力燃料を収納するチャンネルボックスなど原子力用として好適に利用することができる。 (6) The tubular body is for nuclear power.
The tubular body of the present invention is made of a ceramic / ceramic composite material or a SiC / SiC composite material, has heat resistance, and has high strength, so that it can be used for nuclear power such as a channel box for storing nuclear fuel. Can be suitably used.
　本発明の管状体によれば、マンドレルの軸線に対する巻き角度が異なる複数層のセラミック繊維層あるいはＳｉＣ繊維層を有している。このため、管状体にかかる様々な方向の力に対し、いずれかのセラミック繊維層あるいはＳｉＣ繊維層に張力がかかるように配置される。このため、高強度の管状体を得ることができる。 The tubular body of the present invention has a plurality of ceramic fiber layers or SiC fiber layers having different winding angles with respect to the mandrel axis. For this reason, it arrange | positions so that tension | tensile_strength may be applied to any ceramic fiber layer or SiC fiber layer with respect to the force of the various directions concerning a tubular body. For this reason, a high intensity | strength tubular body can be obtained.
　本発明の管状体によれば、複数層のセラミック繊維層あるいはＳｉＣ繊維層は、隙間をＣＶＤ－ＳｉＣによって充填されるので、繊維どうしを強く結びつけることができる。このため高強度の管状体を得ることができる。
　また、管状体の長手方向の辺は、Ｒ面を有しているので、セラミック繊維あるいはＳｉＣ繊維が緩やかに曲がり、延びる側の繊維表面にかかる張力を小さくすることができる。さらにセラミック繊維層あるいはＳｉＣ繊維層は、最外層のセラミック繊維層あるいはＳｉＣ繊維層が、最外層セラミック繊維層直下あるいは最外層ＳｉＣ繊維層直下のセラミック繊維層あるいはＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。このため、繊維の毛羽立ちが少なく、ＣＶＤによって形成されるマトリックスは、毛羽立ちしたＳｉＣ繊維への付着が少なく、ピンホールの少ないＳｉＣ／ＳｉＣ複合材よりなる管状体を得ることができる。 According to the tubular body of the present invention, the plurality of ceramic fiber layers or SiC fiber layers are filled with CVD-SiC in the gaps, so that the fibers can be strongly connected. For this reason, a high strength tubular body can be obtained.
Further, since the longitudinal side of the tubular body has an R surface, the ceramic fiber or the SiC fiber bends gently, and the tension applied to the fiber surface on the extending side can be reduced. Further, the ceramic fiber layer or the SiC fiber layer is wound around the mandrel axis more than the ceramic fiber layer or the SiC fiber layer of the outermost layer directly under the outermost layer of the ceramic fiber layer or directly under the outermost SiC fiber layer. The angle is small. For this reason, the matrix formed by CVD with few fiber fluffs can obtain the tubular body which consists of SiC / SiC composite material with few adhesion to the fluffed SiC fiber, and few pinholes.
本発明の実施形態１の管状体の製造方法の工程フロー図Process flow figure of manufacturing method of tubular body of Embodiment 1 of the present invention 本発明の実施形態１の製造に用いるマンドレルの斜視図The perspective view of the mandrel used for manufacture of Embodiment 1 of this invention 本発明の実施形態１の管状体の巻回工程の詳細工程フロー図The detailed process flow figure of the winding process of the tubular body of Embodiment 1 of this invention 本発明の実施形態１の管状体の外観写真を表す図面Drawing showing the appearance photograph of the tubular body of Embodiment 1 of the present invention 本発明の実施形態１の管状体の断面図Sectional drawing of the tubular body of Embodiment 1 of this invention
　本明細書は、ＳｉＣ繊維と、ＣＶＤ－ＳｉＣのマトリックスにより構成されたＳｉＣ／ＳｉＣ複合材を中心に説明するが、セラミック繊維と、セラミック－ＣＶＤのマトリックスよりなるセラミック／セラミック複合材についても作用効果は同一である。ＳｉＣ繊維はセラミック繊維に対応し、ＣＶＤ－ＳｉＣは、セラミック－ＣＶＤに対応し、置き換えて説明可能である。
　セラミック繊維としては、ＳｉＣ、チタンシリコンカーバイド、アルミナ、ＴａＣ、ＴａＮ、ＳｉＯ２などの繊維が挙げられ特に限定されない。ＣＶＤ－ＳｉＣとしては、ＳｉＣ、チタンシリコンカーバイド、アルミナ、ＴａＣ、ＴａＮ、ＳｉＯ２などが挙げられる。また、セラミック繊維、セラミック－ＣＶＤの組合せについては特に限定されない。 This specification mainly describes a SiC / SiC composite material composed of a SiC fiber and a CVD-SiC matrix. However, the present invention is also effective for a ceramic / ceramic composite material composed of a ceramic fiber and a ceramic-CVD matrix. Are the same. The SiC fiber corresponds to the ceramic fiber, and the CVD-SiC corresponds to the ceramic-CVD and can be described by being replaced.
The ceramic fibers, SiC, not titanium silicon carbide, alumina, TaC, TaN, particularly include fibers such as SiO 2 limited. Examples of CVD-SiC include SiC, titanium silicon carbide, alumina, TaC, TaN, and SiO 2 . Further, the combination of ceramic fiber and ceramic-CVD is not particularly limited.
　本明細書において、マンドレルの軸線とは、マンドレルの長手方向の中心軸である。
　本明細書において、マンドレルの軸線に対する巻き角度とは、ＳｉＣ繊維がマンドレルの軸線に平行な線と交わる角度である。０度の場合、ＳｉＣ繊維はマンドレルの長手方向に巻回され、９０度の場合、マンドレルを周回するように巻回される。 In the present specification, the axis of the mandrel is the central axis in the longitudinal direction of the mandrel.
In the present specification, the winding angle with respect to the axis of the mandrel is an angle at which the SiC fiber intersects with a line parallel to the axis of the mandrel. In the case of 0 degrees, the SiC fiber is wound in the longitudinal direction of the mandrel, and in the case of 90 degrees, the SiC fiber is wound around the mandrel.
　以下本発明の管状体について説明する。 Hereinafter, the tubular body of the present invention will be described.
　本発明の管状体は、複数層のセラミック繊維層と、前記複数層のセラミック繊維層を被覆する繊維被覆層と、前記セラミック繊維層の隙間を充填するとともに外表面を構成するＣＶＤ－セラミック層とからなるセラミック／セラミック複合材からなる多角形の管状体であって、前記管状体の長手方向の辺は、Ｒ面を有し、前記セラミック繊維層は、最外層のセラミック繊維層が、前記最外層セラミック繊維層直下のセラミック繊維層よりもマンドレルの軸線に対する巻き角度が小さい。 The tubular body of the present invention includes a plurality of ceramic fiber layers, a fiber coating layer that covers the plurality of ceramic fiber layers, a CVD-ceramic layer that fills a gap between the ceramic fiber layers and forms an outer surface. A polygonal tubular body made of a ceramic / ceramic composite material, wherein a longitudinal side of the tubular body has an R surface, and the ceramic fiber layer is an outermost ceramic fiber layer. The winding angle with respect to the axis of the mandrel is smaller than that of the ceramic fiber layer immediately below the outer ceramic fiber layer.
　本発明の管状体は、複数層のＳｉＣ繊維層と、前記複数層のＳｉＣ繊維層を被覆する繊維被覆層と、前記ＳｉＣ繊維層の隙間を充填するとともに外表面を構成するＣＶＤ－ＳｉＣ層とからなるＳｉＣ／ＳｉＣ複合材からなる多角形の管状体であって、前記管状体の長手方向の辺は、Ｒ面を有し、前記ＳｉＣ繊維層は、最外層のＳｉＣ繊維層が、前記最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。 The tubular body of the present invention includes a plurality of SiC fiber layers, a fiber coating layer that covers the plurality of SiC fiber layers, a CVD-SiC layer that fills a gap between the SiC fiber layers and constitutes an outer surface. A polygonal tubular body made of a SiC / SiC composite material, wherein the longitudinal side of the tubular body has an R surface, and the SiC fiber layer is the outermost SiC fiber layer. The winding angle with respect to the axis of the mandrel is smaller than that of the SiC fiber layer immediately below the outer SiC fiber layer.
　本発明の管状体によれば、マンドレルの軸線に対する巻き角度が異なる複数層のセラミック繊維層あるいはＳｉＣ繊維層を有している。このため、管状体にかかる様々な方向の力に対し、いずれかのセラミック繊維層あるいはＳｉＣ繊維層に張力がかかるように配置される。このため、高強度の管状体を得ることができる。 The tubular body of the present invention has a plurality of ceramic fiber layers or SiC fiber layers having different winding angles with respect to the mandrel axis. For this reason, it arrange | positions so that tension | tensile_strength may be applied to any ceramic fiber layer or SiC fiber layer with respect to the force of the various directions concerning a tubular body. For this reason, a high intensity | strength tubular body can be obtained.
　本発明の管状体によれば、複数層のセラミック繊維層あるいはＳｉＣ繊維層は、隙間をＣＶＤ－ＳｉＣによって充填されるので、繊維どうしを強く結びつけることができる。このため高強度の管状体を得ることができる。
　また、管状体の長手方向の辺は、Ｒ面を有しているので、セラミック繊維層あるいはＳｉＣ繊維が緩やかに曲がり、延びる側の繊維表面にかかる張力を小さくすることができる。さらにセラミック繊維層あるいはＳｉＣ繊維層は、最外層のセラミック繊維層あるいはＳｉＣ繊維層が、最外層セラミック繊維層あるいは最外層ＳｉＣ繊維層直下のセラミック繊維層あるいはＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。このため、繊維の毛羽立ちが少なく、ＣＶＤによって形成されるマトリックスは、毛羽立ちしたセラミック繊維層あるいはＳｉＣ繊維への付着が少なく、ピンホールの少ないＳｉＣ／ＳｉＣ複合材よりなる管状体を得ることができる。 According to the tubular body of the present invention, the plurality of ceramic fiber layers or SiC fiber layers are filled with CVD-SiC in the gaps, so that the fibers can be strongly connected. For this reason, a high strength tubular body can be obtained.
Further, since the side in the longitudinal direction of the tubular body has an R surface, the ceramic fiber layer or the SiC fiber bends gently, and the tension applied to the fiber surface on the extending side can be reduced. Further, the ceramic fiber layer or SiC fiber layer has an outermost ceramic fiber layer or SiC fiber layer winding angle with respect to the mandrel axis more than the ceramic fiber layer or SiC fiber layer immediately below the outermost ceramic fiber layer or SiC fiber layer. Is small. For this reason, the matrix formed by CVD with few fiber fluffing can obtain the tubular body which consists of a SiC / SiC composite material with few pinholes with few adhesion to the fluffed ceramic fiber layer or SiC fiber.
　本発明の管状体は、以下の態様であることが望ましい。
（１）前記最外層のセラミック繊維層またはＳｉＣ繊維層は、前記マンドレルの軸線に対する巻き角度が３０～６０度である。
　本発明の管状体は、最外層のセラミック繊維層あるいはＳｉＣ繊維層のマンドレルの軸線に対する巻き角度が、３０度以上であると、最外層のセラミック繊維層あるいはＳｉＣ繊維層が管状体に強固に巻き付けられるので、セラミック繊維層あるいはＳｉＣ繊維層の剥離しにくい管状体を構成することができる。最外層のセラミック繊維層あるいはＳｉＣ繊維層のマンドレルの軸線に対する巻き角度が、６０度以下であると、マンドレルの長手方向の辺に沿って曲げられるセラミック繊維あるいはＳｉＣ繊維の曲げの曲率半径を大きくする効果が発揮され、歪みに伴う応力を緩和することができ強固な管状体を得ることができる。 The tubular body of the present invention is desirably in the following manner.
(1) The winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 to 60 degrees.
In the tubular body of the present invention, when the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 degrees or more, the outermost ceramic fiber layer or SiC fiber layer is firmly wound around the tubular body. Therefore, a tubular body in which the ceramic fiber layer or the SiC fiber layer is difficult to peel can be formed. When the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the mandrel axis is 60 degrees or less, the radius of curvature of the bending of the ceramic fiber or SiC fiber bent along the longitudinal side of the mandrel is increased. The effect is exhibited, the stress accompanying the strain can be relaxed, and a strong tubular body can be obtained.
（２）前記管状体は、断面が四角形である。
　四角形の管状体は、複数の管状体を規則的に配列することができ、かつ、管状体の内部に様々なものを収納することができ空間を有効に利用することができる。 (2) The tubular body has a quadrangular cross section.
In the rectangular tubular body, a plurality of tubular bodies can be regularly arranged, and various things can be stored inside the tubular body, so that the space can be used effectively.
（３）前記Ｒ面の曲率半径は、５～２０ｍｍである。
　Ｒ面の曲率半径が、５ｍｍ以上であると、Ｒ面に沿って曲がるセラミック繊維あるいはＳｉＣ繊維にかかる応力を緩和することができる。Ｒ面の曲率半径が、２０ｍｍ以下であると、Ｒ面によってできる利用できない空間を少なくすることができる。 (3) The radius of curvature of the R surface is 5 to 20 mm.
When the radius of curvature of the R plane is 5 mm or more, the stress applied to the ceramic fiber or SiC fiber bent along the R plane can be relaxed. When the radius of curvature of the R surface is 20 mm or less, it is possible to reduce the space that cannot be used by the R surface.
（４）前記セラミック繊維層または前記ＳｉＣ繊維層は、繊維直径が５～２０μｍのセラミック繊維で構成される。
　セラミック繊維の繊維直径が５μｍ以上であると繊維表面に発生する微少な傷などの欠陥の影響を小さくすることができ、折れにくくすることができる。セラミック繊維の繊維直径が２０μｍ以下であると、曲げに伴って延びる側の外表面に発生する張力を抑制することができ、折れにくくすることができ強固な管状体を得ることができる。 (4) The ceramic fiber layer or the SiC fiber layer is composed of ceramic fibers having a fiber diameter of 5 to 20 μm.
When the fiber diameter of the ceramic fiber is 5 μm or more, the influence of defects such as minute scratches generated on the fiber surface can be reduced, and the ceramic fiber can be made difficult to break. When the fiber diameter of the ceramic fiber is 20 μm or less, the tension generated on the outer surface on the side extending along with the bending can be suppressed, and it is possible to obtain a strong tubular body that can be hardly broken.
（５）前記繊維被覆層は、金属元素、シリコン、炭素、ホウ素から選択される１または２以上の元素を含有する。
　これらの元素からなる繊維被覆層がＳｉＣ繊維の表面に有することによって、セラミック繊維あるいはＳｉＣ繊維とマトリックスとの界面に異質な物質を介在させることができる。繊維被覆層が、ＣＶＤ－ＳｉＣからなるマトリックスとセラミック繊維あるいはＳｉＣ繊維との界面に介在することにより、マトリックスからのクラックの伸展を抑制する作用がある。 (5) The fiber coating layer contains one or more elements selected from metal elements, silicon, carbon, and boron.
By having the fiber coating layer made of these elements on the surface of the SiC fiber, a foreign substance can be interposed at the interface between the ceramic fiber or the SiC fiber and the matrix. When the fiber coating layer is interposed at the interface between the CVD-SiC matrix and the ceramic fiber or SiC fiber, there is an action of suppressing the extension of cracks from the matrix.
（６）前記管状体は、原子力用である。
　本発明の管状体は、セラミック／セラミック複合材あるいはＳｉＣ／ＳｉＣ複合材で構成され、耐熱性を有している上に、高い強度を備えているので、原子力燃料を収納するチャンネルボックスなど原子力用として好適に利用することができる。 (6) The tubular body is for nuclear power.
The tubular body of the present invention is made of a ceramic / ceramic composite material or a SiC / SiC composite material, has heat resistance, and has high strength, so that it can be used for nuclear power such as a channel box for storing nuclear fuel. Can be suitably used.
　以下本発明の管状体を得るための製造方法について説明する。
　本発明の管状体の製造方法は、長手方向の辺にＲ面形状部を有する多角形のマンドレルにＳｉＣ繊維を巻回し、前記マンドレルの軸線に対する巻き角度の異なる複数層のＳｉＣ繊維層が積層された巻回体を得る巻回工程と、前記巻回体にＳｉＣ－ＣＶＤを被覆し、被覆体を形成するＣＶＤ工程と、前記被覆体から前記マンドレルを除去するマンドレル除去工程と、からなり、前記各ＳｉＣ繊維層は、最外層のＳｉＣ繊維層が、前記最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりも前記マンドレルの軸線に対する巻き角度が小さいことを特徴とする。 Hereinafter, a production method for obtaining the tubular body of the present invention will be described.
In the method for manufacturing a tubular body of the present invention, SiC fibers are wound around a polygonal mandrel having an R-shaped portion on the longitudinal side, and a plurality of SiC fiber layers having different winding angles with respect to the axis of the mandrel are laminated. A winding process for obtaining a wound body, a CVD process for coating the wound body with SiC-CVD and forming a covering body, and a mandrel removing process for removing the mandrel from the covering body, Each SiC fiber layer is characterized in that the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
　ＳｉＣ繊維は高強度、高弾性の繊維であるため、引っ張りに対しては高強度を発揮する一方、歪みに対しては発生する応力が大きく、折れやすい性質を持っている。このため、鋭い曲げ加工が必要な多角形の管状体では、コーナー部分で繊維が折れ、毛羽立ちができやすくなる。本発明では、マンドレルの長手方向の辺にＲ面を有しているので、ＳｉＣ繊維の曲げに伴う応力を小さくでき折れにくくすることができる。 Since SiC fiber is a high strength and high elasticity fiber, it exhibits a high strength against tension, but has a large amount of stress generated against strain and is easy to break. For this reason, in a polygonal tubular body that requires sharp bending, fibers are broken at the corner portion, and fluffing is likely to occur. In this invention, since it has R surface in the side of the longitudinal direction of a mandrel, the stress accompanying the bending of a SiC fiber can be made small and it cannot be broken easily.
　また、ＳｉＣ繊維をマンドレルの軸線に対する巻き角度が小さくなるように、マンドレルに巻回することにより、ＳｉＣ繊維の曲げの曲率半径をより大きくし、曲げに伴う応力を緩和することができる。さらに、マンドレルの軸線に対する巻き角度が小さいＳｉＣ繊維層を最外層に配置することにより、最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりも折れにくくできる。つまり毛羽立ちし易いＳｉＣ繊維層を、毛羽立ちしにくいＳｉＣ繊維層で覆い、毛羽立ちの発生を抑えることができる。 Further, by winding the SiC fiber around the mandrel so that the winding angle with respect to the axis of the mandrel becomes small, the curvature radius of the bending of the SiC fiber can be further increased and the stress accompanying the bending can be reduced. Furthermore, by arranging the SiC fiber layer having a small winding angle with respect to the axis of the mandrel in the outermost layer, it can be more difficult to break than the SiC fiber layer immediately below the outermost SiC fiber layer. That is, it is possible to cover the SiC fiber layer that is easily fluffed with the SiC fiber layer that is difficult to fluff, and to suppress the occurrence of fluff.
　また本発明の管状体は、マンドレルの軸線に対する巻き角度が異なる複数層のＳｉＣ繊維層を有している。このため、管状体にかかる様々な方向の力に対し、いずれかのＳｉＣ繊維層に張力がかかるように配置される。このため、高強度の管状体を得ることができる。 The tubular body of the present invention has a plurality of SiC fiber layers having different winding angles with respect to the axis of the mandrel. For this reason, it arrange | positions so that tension | tensile_strength may be applied to any SiC fiber layer with respect to the force of the various directions concerning a tubular body. For this reason, a high intensity | strength tubular body can be obtained.
　さらに、複数層のＳｉＣ繊維層は、隙間をＣＶＤ－ＳｉＣによって充填されるので、繊維どうしを強く結びつけることができる。 Furthermore, since the plurality of SiC fiber layers are filled with CVD-SiC in the gaps, the fibers can be strongly connected.
　さらに本発明の管状体は、以下のように製造されることが望ましい。
（１）前記巻回工程と、前記ＣＶＤ工程との間に、前記巻回体にコーティング材を塗布後、焼成するコーティング工程をさらに有する。
　ＣＶＤ工程では高温に曝されるため、熱膨張差でＳｉＣ繊維に負担が掛かり毛羽立ちの発生原因となりやすい。本発明では、ＳｉＣ繊維の毛羽立ちの発生しやすいＣＶＤ工程の前に、コーティング工程を加えることでＳｉＣ繊維に繊維被覆層を形成するとともにＳｉＣ繊維を互いに結び付けているので、毛羽立ちの発生を抑えることができる。
　ＣＶＤ工程の原料ガスを流す段階で毛羽立ちがあると、毛羽立ちにもＣＶＤ－ＳｉＣが沈着し、原料ガスが巻回体の内部に充分行き渡らず、管状体にピンホールなど欠陥ができやすくなるが、このような構成にすることにより、一様にＣＶＤ－ＳｉＣが被覆され、毛羽立ちを原因とする欠陥の発生を抑止することができる。 Furthermore, it is desirable that the tubular body of the present invention is manufactured as follows.
(1) Between the winding step and the CVD step, the method further includes a coating step of baking after applying a coating material to the wound body.
Since the CVD process is exposed to a high temperature, the SiC fiber is burdened by the difference in thermal expansion, and is likely to cause fluffing. In the present invention, since a fiber coating layer is formed on the SiC fiber by adding a coating process before the CVD process in which SiC fiber is likely to fluff, and the SiC fibers are bound to each other, the occurrence of fluff can be suppressed. it can.
If there is fuzz at the stage of flowing the source gas in the CVD process, CVD-SiC is deposited on the fuzz and the source gas does not spread sufficiently inside the wound body, making it easy to make defects such as pinholes in the tubular body, With such a configuration, the CVD-SiC is uniformly coated, and generation of defects due to fluffing can be suppressed.
　また、コーティング工程により、ＳｉＣ繊維の表面に繊維被覆層を形成する。繊維被覆層はＣＶＤ－ＳｉＣによるマトリックスとＳｉＣ繊維との界面に形成されるので、マトリックスから伸展するクラックをＳｉＣ繊維に伝達しないように応力を分散することができる。
　これら作用により、高強度のＳｉＣ／ＳｉＣ複合材よりなる管状体を得ることができる。 Moreover, a fiber coating layer is formed on the surface of the SiC fiber by a coating process. Since the fiber coating layer is formed at the interface between the CVD-SiC matrix and the SiC fiber, the stress can be dispersed so that cracks extending from the matrix are not transmitted to the SiC fiber.
By these actions, a tubular body made of a high-strength SiC / SiC composite material can be obtained.
（２）前記最外層のセラミック繊維層またはＳｉＣ繊維層は、前記マンドレルの軸線に対する巻き角度が３０～６０度である。
　最外層のセラミック繊維層またはＳｉＣ繊維層のマンドレルの軸線に対する巻き角度が、３０度以上であると、最外層のセラミック繊維層またはＳｉＣ繊維層が管状体に強固に巻き付けられるので、ＳｉＣ繊維層の剥離しにくい管状体を構成することができる。最外層のセラミック繊維層またはＳｉＣ繊維層のマンドレルの軸線に対する巻き角度が、６０度以下であると、マンドレルの長手方向の辺に沿って曲げられるセラミック繊維またはＳｉＣ繊維の曲げの曲率半径を大きくすることができ、歪みに伴う応力を緩和することができる。 (2) The winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 to 60 degrees.
When the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 30 degrees or more, the outermost ceramic fiber layer or SiC fiber layer is firmly wound around the tubular body. A tubular body that is difficult to peel can be formed. When the winding angle of the outermost ceramic fiber layer or SiC fiber layer with respect to the axis of the mandrel is 60 degrees or less, the radius of curvature of the bending of the ceramic fiber or SiC fiber bent along the longitudinal side of the mandrel is increased. And stress associated with strain can be relaxed.
（３）前記管状体は、断面が四角形である。
　四角形の管状体であれば、複数の管状体を規則的に配列することができる上に、管状体の内部に様々なものを収納することができ空間を有効に利用できる。 (3) The tubular body has a quadrangular cross section.
In the case of a rectangular tubular body, a plurality of tubular bodies can be regularly arranged, and various things can be stored inside the tubular body, so that the space can be used effectively.
（４）前記Ｒ面形状部の曲率半径は、５～２０ｍｍである。
　本発明の管状体は、Ｒ面形状部の曲率半径が、５ｍｍ以上であると、Ｒ面に沿って曲がるＳｉＣ繊維にかかる応力を緩和することができる。Ｒ面形状部の曲率半径は、２０ｍｍ以下であると、Ｒ面形状部によってできる利用できない空間を少なくすることができる。 (4) The radius of curvature of the R-surface shaped part is 5 to 20 mm.
In the tubular body of the present invention, when the radius of curvature of the R-plane shape portion is 5 mm or more, the stress applied to the SiC fiber that is bent along the R-plane can be relaxed. When the radius of curvature of the R-surface shape portion is 20 mm or less, it is possible to reduce an unusable space that can be generated by the R-surface shape portion.
（５）前記セラミック繊維層または前記ＳｉＣ繊維層は、繊維直径が５～２０μｍのセラミック繊維で構成される。
　セラミック繊維の繊維直径が５μｍ以上であると繊維表面に発生する微少な傷などの欠陥の影響を小さくすることができ、折れにくくすることができる。セラミック繊維の繊維直径が２０μｍ以下であると、曲げに伴って延びる側の外表面に発生する張力を抑制することができ、折れにくくすることができる。 (5) The ceramic fiber layer or the SiC fiber layer is composed of ceramic fibers having a fiber diameter of 5 to 20 μm.
When the fiber diameter of the ceramic fiber is 5 μm or more, the influence of defects such as minute scratches generated on the fiber surface can be reduced, and the ceramic fiber can be made difficult to break. When the fiber diameter of the ceramic fiber is 20 μm or less, it is possible to suppress the tension generated on the outer surface on the side extending along with the bending and make it difficult to break.
（６）前記コーティング材は、金属元素、シリコン、炭素、ホウ素から選択される１または２以上の元素を含有する化合物である。
　これらの化合物は、焼成によってＳｉＣ繊維の表面に残留し、繊維被覆層を形成する。繊維被覆層が、ＣＶＤ－ＳｉＣからなるマトリックスとＳｉＣ繊維との界面に介在することにより、マトリックスからのクラックの伸展を抑制する作用がある。 (6) The coating material is a compound containing one or more elements selected from metal elements, silicon, carbon, and boron.
These compounds remain on the surface of the SiC fiber by firing to form a fiber coating layer. Since the fiber coating layer is interposed at the interface between the CVD-SiC matrix and the SiC fibers, it has an action of suppressing the extension of cracks from the matrix.
（７）前記管状体は、原子力用である。
　本発明の管状体は、ＳｉＣ／ＳｉＣ複合材で構成され、耐熱性を有している上に、高い強度を備えているので、原子力燃料を収納するチャンネルボックスなど原子力用として好適に利用することができる。 (7) The tubular body is for nuclear power.
The tubular body of the present invention is composed of a SiC / SiC composite material, has heat resistance, and has high strength, so that it can be suitably used for nuclear power such as a channel box for storing nuclear fuel. Can do.
　本発明の管状体の製造方法の実施形態１について説明する。（図１（ａ）～図１（ｄ））
　実施形態１の管状体の製造方法は、巻回工程（図１（ａ））、コーティング工程（図１（ｂ））、ＣＶＤ工程（図１（ｃ））、マンドレル除去工程（図１（ｄ））とからなる。 Embodiment 1 of the manufacturing method of the tubular body of this invention is demonstrated. (FIG. 1 (a) to FIG. 1 (d))
The manufacturing method of the tubular body of Embodiment 1 includes a winding process (FIG. 1A), a coating process (FIG. 1B), a CVD process (FIG. 1C), and a mandrel removing process (FIG. 1D). )).
＜巻回工程＞図１（ａ）
　本発明の管状体の製造に用いるマンドレルは、ＳｉＣ繊維を巻回したまま焼成、ＣＶＤ処理がされるので耐熱性を有するものであればよく、特に限定されない。例えば、黒鉛、ＳｉＣなどが利用できる。黒鉛としては、等方性黒鉛材などが利用でできる。等方性黒鉛材は、ＳｉＣと熱膨張係数が近いので加熱、冷却の過程で熱歪みが発生しにくい。
　また、黒鉛は後のマンドレル除去工程で、空気酸化させて除去することができる利点もある。 <Winding process> FIG. 1 (a)
The mandrel used in the production of the tubular body of the present invention is not particularly limited as long as it has heat resistance because it is fired and CVD-treated while the SiC fiber is wound. For example, graphite, SiC, etc. can be used. As the graphite, an isotropic graphite material or the like can be used. An isotropic graphite material has a thermal expansion coefficient close to that of SiC, so that thermal distortion is unlikely to occur during heating and cooling.
Further, there is an advantage that graphite can be removed by air oxidation in a later mandrel removal step.
　黒鉛のマンドレル１を回転させながら、複数のＳｉＣ繊維を束ねたストランドの形態で巻回する。ＳｉＣ繊維は特に限定されない。例えば、宇部興産株式会社製ＳｉＣ繊維「チラノＳＡ」を用いることができる。繊維直径は７．５μｍである。
　黒鉛のマンドレル１は、断面が１３０ｍｍの辺の長さの正方形であり、コーナー部分は１０ｍｍのＲ面形状部２がなされている。また、黒鉛のマンドレル１の長さは１０００ｍｍである。図２にそのマンドレルの斜視図を示す。マンドレル１の長手方向の４辺にはＲ面形状部を有している。 While the graphite mandrel 1 is rotated, it is wound in the form of a strand in which a plurality of SiC fibers are bundled. The SiC fiber is not particularly limited. For example, Ube Industries, Ltd. SiC fiber "Tyranno SA" can be used. The fiber diameter is 7.5 μm.
The graphite mandrel 1 is a square having a side length of 130 mm in cross section, and an R-plane shape portion 2 having a 10 mm corner portion. The length of the graphite mandrel 1 is 1000 mm. FIG. 2 shows a perspective view of the mandrel. The four sides in the longitudinal direction of the mandrel 1 have R-shaped portions.
　実施形態１の管状体の巻回工程を、図３を用いて説明する。
　１層目を示す図３（ａ）では、ＳｉＣ繊維をマンドレルの軸線に対し４５度となるように交互に移動させながら巻回する。交互に移動しながら巻回するので、表面に菱形の模様が形成されるヘリカル巻きとなる。
　２層目を示す図３（ｂ）では、マンドレルの軸線に対し０度となるように、複数のＳｉＣ繊維を束ねたストランドの形態で巻回する。
　３層目を示す図３（ｃ）では、マンドレルの軸線に直交するように、複数のＳｉＣ繊維を束ねたストランドの形態で巻回する。このような巻き方は、フープ巻きである。
　４層目を示す図３（ｄ）では、ＳｉＣ繊維をマンドレルの軸線に対し４５度となるように交互に移動させながら巻回する。交互に移動しながら巻回するので、表面に菱形の模様が形成されるヘリカル巻きとなる。
　このように４層のＳｉＣ繊維層を有する巻回体が得られる。 The winding process of the tubular body of Embodiment 1 is demonstrated using FIG.
In FIG. 3A showing the first layer, the SiC fiber is wound while being alternately moved so as to be 45 degrees with respect to the axis of the mandrel. Since it winds while moving alternately, it becomes a helical winding in which a rhombus pattern is formed on the surface.
In FIG.3 (b) which shows the 2nd layer, it winds with the form of the strand which bundled several SiC fiber so that it might become 0 degree | times with respect to the axis line of a mandrel.
In FIG.3 (c) which shows the 3rd layer, it winds with the form of the strand which bundled the several SiC fiber so that it might orthogonally cross the axis line of a mandrel. Such a winding method is hoop winding.
In FIG. 3D showing the fourth layer, the SiC fiber is wound while being alternately moved so as to be 45 degrees with respect to the axis of the mandrel. Since it winds while moving alternately, it becomes a helical winding in which a rhombus pattern is formed on the surface.
In this way, a wound body having four SiC fiber layers is obtained.
　最外層である４層目のＳｉＣ繊維層は、マンドレルの軸線に対し４５度の巻き角度であり、最外層ＳｉＣ繊維層直下の３層目のＳｉＣ繊維層は、マンドレルの軸線に対し９０度の巻き角度である。このような構成にすることにより最外層のＳｉＣ繊維層が、最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい巻回体がえられる。
　長辺にＲ面形状部２を有するマンドレルにＳｉＣ繊維を巻回するので、ＳｉＣ繊維に大きな曲げ応力が加わりにくくすることができる。
　また、３層目のＳｉＣ繊維は、マンドレルの軸線に直交するようにＳｉＣ繊維が巻回されるのでマンドレルのＲ面形状部の曲率半径と同等の曲率半径で巻回される。これに対し、最外層の４層目のマンドレルでは、マンドレルの軸線に対し４５度の角度で巻回されるので、実際巻回されるＳｉＣ繊維の曲率半径は（１／ｃｏｓ４５度）倍、すなわち１．４１倍に緩和され、より折れにくくすることができる。
　このような構成にすることにより、より折れにくくなったＳｉＣ繊維層で最外層が構成されるので、毛羽立ちを効率良く防止することができる。 The fourth SiC fiber layer that is the outermost layer has a winding angle of 45 degrees with respect to the axis of the mandrel, and the third SiC fiber layer immediately below the outermost SiC fiber layer is 90 degrees with respect to the axis of the mandrel. It is a winding angle. With such a configuration, a wound body is obtained in which the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
Since the SiC fiber is wound around the mandrel having the R-shaped portion 2 on the long side, it is possible to make it difficult to apply a large bending stress to the SiC fiber.
Further, since the SiC fiber is wound so that the third-layer SiC fiber is orthogonal to the axis of the mandrel, the SiC fiber is wound with a curvature radius equivalent to the curvature radius of the R-surface shape portion of the mandrel. On the other hand, the mandrel of the fourth outermost layer is wound at an angle of 45 degrees with respect to the axis of the mandrel, so the radius of curvature of the actually wound SiC fiber is (1 / cos 45 degrees), that is, It is relaxed 1.41 times and can be made more difficult to break.
By setting it as such a structure, since the outermost layer is comprised by the SiC fiber layer which became hard to break, fuzzing can be prevented efficiently.
＜コーティング工程＞図１（ｂ）
　次に、巻回体に、コーティング材を塗布した後焼成する。コーティング材としては、金属元素、シリコン、炭素、ホウ素から選択される１または２以上の元素を含有する化合物である。
　実施形態１ではコーティング材として、フェノール樹脂であり、焼成によって、ＳｉＣ繊維の表面に繊維被覆層を形成する。
　これらの化合物は、焼成によってＳｉＣ繊維の表面に残留し、繊維被覆層を形成する。繊維被覆層が、ＣＶＤ－ＳｉＣからなるマトリックスとＳｉＣ繊維との界面に介在することにより、マトリックスからのクラックの伸展を抑制する作用がある。
　コーティング工程は必須ではないが、このようにＳｉＣ／ＳｉＣ複合材を破壊しにくくする効果があるため、管状体の製造方法に用いることが望ましい。
　他のコーティング材としては、例えば、ポリカルボシラン、ポリオルガノボロンシラザン、フラン樹脂などの有機物、有機金属化合物、ナノシリカなどのセラミック微細粒子などが利用できる。
　焼成は、例えば４００～１０００℃で処理することができる。焼成雰囲気は、形成する繊維被覆層の形態によって適宜選択することができ、例えば、カーボン系の繊維被覆層の場合には還元性雰囲気、酸化物系の繊維被覆層には酸化性雰囲気とすることにより、望ましい繊維被覆層を得ることができる。 <Coating process> FIG. 1 (b)
Next, the coating material is applied to the wound body and then fired. The coating material is a compound containing one or more elements selected from metal elements, silicon, carbon, and boron.
In the first embodiment, the coating material is a phenol resin, and a fiber coating layer is formed on the surface of the SiC fiber by firing.
These compounds remain on the surface of the SiC fiber by firing to form a fiber coating layer. Since the fiber coating layer is interposed at the interface between the CVD-SiC matrix and the SiC fibers, it has an action of suppressing the extension of cracks from the matrix.
The coating process is not essential, but it is desirable to use the method for manufacturing a tubular body because it has the effect of making the SiC / SiC composite material difficult to break.
Examples of other coating materials that can be used include organic substances such as polycarbosilane, polyorganoboronsilazane, furan resin, organometallic compounds, and ceramic fine particles such as nano silica.
Firing can be performed at 400 to 1000 ° C., for example. The firing atmosphere can be appropriately selected depending on the form of the fiber coating layer to be formed. For example, in the case of a carbon-based fiber coating layer, a reducing atmosphere is used, and in the case of an oxide-based fiber coating layer, an oxidizing atmosphere is used. Thus, a desired fiber coating layer can be obtained.
　＜ＣＶＤ工程＞図１（ｃ）
　こうして得られた巻回体を、ＣＶＤ炉に入れ、ＣＶＤ－ＳｉＣにより被覆する。
　成膜温度は、例えば１０００～１８００℃が利用できる。原料ガスは特に限定されない。例えば、シランガス／メタンガスの混合ガス、テトラクロロシランガス／メタンガスの混合ガス、メチルトリクロロシラン（ＭＴＳ）などが利用できる。他に炉内分圧を調整するための水素ガスなどを適宜利用することができる。
　ＣＶＤの形式は特に限定されないが、炉内のヒーターの輻射で炉内全体を暖めるホットウォール型、マンドレル内部に組み込まれたヒーターにより、巻回体のみを暖めるコールドウォール型のいずれでも利用することができる。コールドウォール型を用いた場合には、原料ガスを供給するノズルに被膜は形成されにくいので、効率良く成膜することができ、厚い被膜を容易に得ることができる。
　なお、ＣＶＤ－ＳｉＣは、ＳｉＣ繊維間を充填するだけではなく、さらに沈積することによって、ＣＶＤ－ＳｉＣのみからなる表層を有している。 <CVD process> FIG. 1 (c)
The wound body thus obtained is placed in a CVD furnace and covered with CVD-SiC.
The film forming temperature can be 1000 to 1800 ° C., for example. The source gas is not particularly limited. For example, a mixed gas of silane gas / methane gas, a mixed gas of tetrachlorosilane gas / methane gas, methyltrichlorosilane (MTS), or the like can be used. In addition, hydrogen gas or the like for adjusting the partial pressure in the furnace can be used as appropriate.
The type of CVD is not particularly limited, but it can be used in either a hot wall type that heats the entire furnace by radiation of the heater in the furnace, or a cold wall type that heats only the wound body by a heater built into the mandrel. it can. When the cold wall type is used, it is difficult to form a film on the nozzle that supplies the source gas, so that the film can be efficiently formed and a thick film can be easily obtained.
Note that CVD-SiC not only fills the space between the SiC fibers but also deposits it to have a surface layer made of only CVD-SiC.
＜マンドレル除去工程＞図１（ｄ）
　こうして得られたマンドレルを除去することにより、四角形のＳｉＣ／ＳｉＣ複合材よりなる管状体を得ることができる。
　マンドレルの除去の方法は、特に限定されない。機械的に切削加工して除去する切削法、酸化雰囲気炉で燃焼させる燃焼法、油圧など外部からの力で引き抜く引き抜き法など、どのような方法でも利用でき、これらを併用しても良い。
　さらに、管状体の両端を切断し、形状を整える。 <Mandrel removal process> FIG. 1 (d)
By removing the mandrel thus obtained, a tubular body made of a square SiC / SiC composite material can be obtained.
The method for removing the mandrel is not particularly limited. Any method can be used, such as a cutting method that is mechanically cut and removed, a combustion method that burns in an oxidizing atmosphere furnace, or a pulling method that is pulled out by an external force such as hydraulic pressure, and these methods may be used in combination.
Furthermore, the both ends of the tubular body are cut to adjust the shape.
　次に得られた実施形態１の管状体について説明する。図４は実施形態１の製造方法で得られた管状体の外観写真を表す図面である。ヘリカル巻きの特徴である菱形の模様を表面に有している。図５（ａ）～図５（ｃ）は、実施形態１の管状体の断面図である。
　ＳｉＣ繊維層４と、ＣＶＤ－ＳｉＣからなるマトリックス５を有している。ＣＶＤ－ＳｉＣからなるマトリックス５は、繊維間を充填するのみならず、さらに沈積し、ＣＶＤ－ＳｉＣのみからなる表層部を有している。
　このようにして得られた管状体１０は、複数層のＳｉＣ繊維層４と、複数層のＳｉＣ繊維層４を被覆する繊維被覆層８と、ＳｉＣ繊維層４の隙間を充填するとともに外表面を構成するＣＶＤ－ＳｉＣ５とからなるＳｉＣ／ＳｉＣ複合材からなる多角形の管状体１０であって、管状体１０の長手方向の辺は、Ｒ面６を有し、ＳｉＣ繊維層４は、最外層のＳｉＣ繊維層が、最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。 Next, the obtained tubular body of Embodiment 1 will be described. FIG. 4 is a drawing showing an external appearance photograph of the tubular body obtained by the manufacturing method of the first embodiment. It has a diamond-shaped pattern on the surface that is characteristic of helical winding. FIGS. 5A to 5C are cross-sectional views of the tubular body of the first embodiment.
It has a SiC fiber layer 4 and a matrix 5 made of CVD-SiC. The matrix 5 made of CVD-SiC not only fills between the fibers, but further deposits and has a surface layer portion made only of CVD-SiC.
The tubular body 10 thus obtained has a plurality of SiC fiber layers 4, a fiber coating layer 8 that covers the plurality of SiC fiber layers 4, and a gap between the SiC fiber layers 4 and an outer surface. A polygonal tubular body 10 made of a SiC / SiC composite material composed of CVD-SiC 5 constituting, the side of the tubular body 10 in the longitudinal direction has an R surface 6, and the SiC fiber layer 4 is an outermost layer. The SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
　また実施形態１の管状体１０は、マンドレルの軸線に対する巻き角度が異なる複数層のＳｉＣ繊維層４を有している。このため、管状体１０にかかる様々な方向の力に対し、いずれかのＳｉＣ繊維層４に張力がかかるように配置される。 Moreover, the tubular body 10 of Embodiment 1 has a plurality of SiC fiber layers 4 having different winding angles with respect to the mandrel axis. For this reason, it arrange | positions so that tension | tensile_strength may be applied to any SiC fiber layer 4 with respect to the force of the various directions concerning the tubular body 10. FIG.
　複数層のＳｉＣ繊維層４は、隙間をＣＶＤ－ＳｉＣ５によって充填されるので、繊維どうしを強く結びつくことができる。このため高強度の管状体１０を得ることができる。
　また、管状体１０の長手方向の辺は、Ｒ面６を有しているので、ＳｉＣ繊維が緩やかに曲がり、延びる側の繊維表面にかかる張力を小さくすることができる。ＳｉＣ繊維層４は、最外層のＳｉＣ繊維層が、最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さい。このため、繊維の毛羽立ちが少なく、ＣＶＤによって形成されるマトリックスは、毛羽立ちしたＳｉＣ繊維への付着が少なく、ピンホールの少ないＳｉＣ／ＳｉＣ複合材よりなる管状体を得ることができる。 In the plurality of SiC fiber layers 4, the gaps are filled with CVD-SiC 5, so that the fibers can be strongly connected. For this reason, the high strength tubular body 10 can be obtained.
Further, since the side in the longitudinal direction of the tubular body 10 has the R surface 6, the SiC fiber bends gently, and the tension applied to the extending fiber surface can be reduced. In SiC fiber layer 4, the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer. For this reason, the matrix formed by CVD with few fiber fluffs can obtain the tubular body which consists of SiC / SiC composite material with few adhesion to the fluffed SiC fiber, and few pinholes.
　本出願は、2014年7月2日出願の日本国特許出願（特願2014-137017）に基づくものであり、それらの内容はここに参照として取り込まれる。 This application is based on a Japanese patent application filed on July 2, 2014 (Japanese Patent Application No. 2014-137017), the contents of which are incorporated herein by reference.
　原子力用途の燃料集合体材料にとして用いられる薄肉長尺角筒、薄肉長尺円筒などの様々な形状にも利用することができる。 It can also be used in various shapes such as thin long rectangular tubes and thin long cylinders used as fuel assembly materials for nuclear applications.
１　マンドレル
２　Ｒ面形状部
３　マンドレルの軸線
４　ＳｉＣ繊維層
５　ＣＶＤ－ＳｉＣ（マトリックス）
６　Ｒ面
７　ＳｉＣ繊維
８　繊維被覆層
１０　管状体 DESCRIPTION OF SYMBOLS 1 Mandrel 2 R surface shape part 3 Mandrel axis 4 SiC fiber layer 5 CVD-SiC (matrix)
6 R face 7 SiC fiber 8 Fiber coating layer 10 Tubular body

Claims (8)

  1. 　複数層のセラミック繊維層と、前記複数層のセラミック繊維層を被覆する繊維被覆層と、前記セラミック繊維層の隙間を充填するとともに外表面を構成するＣＶＤ－セラミック層とからなるセラミック／セラミック複合材からなる多角形の管状体であって、
    　前記管状体の長手方向の辺は、Ｒ面を有し、
    　前記セラミック繊維層は、最外層のセラミック繊維層が、前記最外層セラミック繊維層直下のセラミック繊維層よりもマンドレルの軸線に対する巻き角度が小さいことを特徴とする多角形の管状体。     A ceramic / ceramic composite material comprising: a plurality of ceramic fiber layers; a fiber coating layer for covering the plurality of ceramic fiber layers; and a CVD-ceramic layer that fills a gap between the ceramic fiber layers and constitutes an outer surface A polygonal tubular body consisting of
    The longitudinal side of the tubular body has an R-plane,
    The ceramic fiber layer is a polygonal tubular body characterized in that the outermost ceramic fiber layer has a smaller winding angle with respect to the axis of the mandrel than the ceramic fiber layer immediately below the outermost ceramic fiber layer.
  2. 　複数層のＳｉＣ繊維層と、前記複数層のＳｉＣ繊維層を被覆する繊維被覆層と、前記ＳｉＣ繊維層の隙間を充填するとともに外表面を構成するＣＶＤ－ＳｉＣ層とからなるＳｉＣ／ＳｉＣ複合材からなる多角形の管状体であって、
    　前記管状体の長手方向の辺は、Ｒ面を有し、
    　前記ＳｉＣ繊維層は、最外層のＳｉＣ繊維層が、前記最外層ＳｉＣ繊維層直下のＳｉＣ繊維層よりもマンドレルの軸線に対する巻き角度が小さいことを特徴とする多角形の管状体。     SiC / SiC composite material comprising a plurality of SiC fiber layers, a fiber coating layer that covers the plurality of SiC fiber layers, and a CVD-SiC layer that fills the gaps between the SiC fiber layers and constitutes the outer surface A polygonal tubular body consisting of
    The longitudinal side of the tubular body has an R-plane,
    The SiC fiber layer is a polygonal tubular body characterized in that the outermost SiC fiber layer has a smaller winding angle with respect to the axis of the mandrel than the SiC fiber layer immediately below the outermost SiC fiber layer.
  3. 　前記最外層のセラミック繊維層またはＳｉＣ繊維層は、前記マンドレルの軸線に対する巻き角度が３０～６０度であることを特徴とする請求項１または請求項２に記載の管状体。 The tubular body according to claim 1 or 2, wherein the outermost ceramic fiber layer or SiC fiber layer has a winding angle of 30 to 60 degrees with respect to the axis of the mandrel.
  4. 　前記管状体は、断面が四角形であることを特徴とする請求項１～請求項３のうちのいずれか１項に記載の管状体。 The tubular body according to any one of claims 1 to 3, wherein the tubular body has a quadrangular cross section.
  5. 　前記Ｒ面の曲率半径は、５～２０ｍｍであることを特徴とする請求項１～請求項４のうちのいずれか１項に記載の管状体。 The tubular body according to any one of claims 1 to 4, wherein a radius of curvature of the R surface is 5 to 20 mm.
  6. 　前記セラミック繊維層または前記ＳｉＣ繊維層は、繊維直径が５～２０μｍのセラミック繊維で構成されることを特徴とする請求項３～請求項５のうちのいずれか１項に記載の管状体。 The tubular body according to any one of claims 3 to 5, wherein the ceramic fiber layer or the SiC fiber layer is made of a ceramic fiber having a fiber diameter of 5 to 20 µm.
  7. 　前記繊維被覆層は、金属元素、シリコン、炭素、ホウ素から選択される１または２以上の元素を含有することを特徴とする請求項１～請求項６のうちのいずれか１項に記載の管状体。 The tubular according to any one of claims 1 to 6, wherein the fiber coating layer contains one or more elements selected from metal elements, silicon, carbon, and boron. body.
  8. 　前記管状体は、原子力用であることを特徴とする請求項１～請求項７のうちのいずれか１項に記載の管状体。 The tubular body according to any one of claims 1 to 7, wherein the tubular body is for nuclear power.
PCT/JP2015/069214 2014-07-02 2015-07-02 Tubular body WO2016002914A1 (en)

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JP2018193259A (en) * 2017-05-15 2018-12-06 株式会社東芝 Continuous fiber-reinforced silicon carbide member, manufacturing method thereof, and nuclear reactor structural member
EP3647043A1 (en) * 2018-11-01 2020-05-06 Admap, Inc. Tubular body containing sic fiber and method for producing the same
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