WO2011114810A1 - 繊維束用無機繊維及びその製造方法、その繊維束用無機繊維から構成される複合材料用無機繊維束、並びにその繊維束で強化されたセラミックス基複合材料 - Google Patents
繊維束用無機繊維及びその製造方法、その繊維束用無機繊維から構成される複合材料用無機繊維束、並びにその繊維束で強化されたセラミックス基複合材料 Download PDFInfo
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Definitions
- the present invention relates to an inorganic fiber for a fiber bundle and a method for producing the same, an inorganic fiber bundle for a composite material composed of the inorganic fiber for the fiber bundle, and a ceramic matrix composite material reinforced with the fiber bundle.
- Ceramic base composite materials reinforced with inorganic fibers are being developed as next-generation heat-resistant materials because of their excellent heat resistance not found in metals and damage tolerance not found in conventional single-phase ceramics.
- the bond at the interface between the reinforcing fiber and the matrix is controlled, and cracks are deflected at the interface when the material breaks, and the breakage progresses while the fiber pulls out. It is a feature.
- a ceramic matrix composite material reinforced with silicon carbide fibers using non-oxide silicon carbide or silicon nitride as a matrix has attracted particular attention.
- Expected uses of these ceramic matrix composite materials include the gas turbine field and the like, and durability under a high temperature and oxidizing atmosphere is required.
- a preform is produced by molding a reinforcing material, such as an inorganic fiber fabric, into a desired shape.
- a sizing agent used to converge the fiber bundle is decomposed and removed in an inert atmosphere such as argon or nitrogen at a high temperature of 600 ° C. or higher, an interface layer for controlling the interface with the matrix is controlled. It is formed on the fiber surface by chemical vapor deposition (CVD method, CVI method).
- CVD method, CVI method chemical vapor deposition
- carbon or boron nitride is mainly selected.
- the matrix is similarly subjected to chemical vapor deposition, or a method of impregnating an inorganic or organic polymer melt or solution as a matrix raw material, followed by firing, and repeating this step if necessary.
- Non-Patent Document 1 in a ceramic matrix composite material of a silicon carbide matrix reinforced with silicon carbide fibers, an interface layer of boron nitride is not uniformly formed at the contact point of the fibers in the fiber bundle. It is shown that when the fiber is subjected to stress in a high temperature / oxidizing atmosphere, the fiber contact point is preferentially oxidized to form an oxide glass layer. It has been pointed out that fibers are firmly bonded by this glass layer, causing stress concentration, causing brittle fracture, and the expected durability cannot be obtained.
- Patent Documents 1 and 2 Non-Patent Document 2
- JP-A-63-59473 Japanese Patent Laid-Open No. 62-299568
- the heat-resistant substances are also decomposed in the sizing agent removal process, interface layer formation process and matrix formation process. Does not remain in the composite material.
- the interface layer forming step where the heat-resistant substance adheres to the fiber surface, the interface layer is not formed on the fiber surface, and fiber pull-out is suppressed at the time of destruction. Does not show energy.
- the heat-resistant substance has a high hardness like inorganic fibers, and also has an irregular shape and an edge shape, so in the process of adhering to the fiber surface or the process of weaving the fibers into a woven fabric, guides, rollers, etc. Due to the friction, the heat-resistant substance damages the fiber and the fiber strength is lowered. Therefore, there is a problem that the strength of the obtained composite material is also lowered.
- the present invention provides a ceramic-based composite material exhibiting sufficient strength and fracture energy, and excellent durability when subjected to stress in a high temperature / oxidizing atmosphere. Suppressing the decrease in fiber strength due to fiber damage during production of inorganic fiber bundles for materials, and avoiding contact between fibers in fiber bundles during production of composite materials, and interfacing with the matrix on the entire fiber surface It is an object to provide an inorganic fiber for a fiber bundle capable of forming a layer, a method for producing the same, an inorganic fiber bundle for a composite material composed of the inorganic fiber for the fiber bundle, and a ceramic matrix composite material reinforced with the fiber bundle To do.
- the present inventors meandered in the longitudinal direction, and made the inorganic fiber having a specific meander pitch and meander width as a fiber bundle. It has been found that the object of the present invention can be achieved.
- the present invention is characterized in that the fiber bundle inorganic fibers constituting the composite material inorganic fiber bundle meander in the longitudinal direction, the meander pitch is 3 to 40 mm, and the meander width is 0.1 to 5 mm.
- the present invention relates to inorganic fibers for fiber bundles.
- the elemental composition is Si: 45 to 60% by mass, Ti or Zr: 0.2 to 5% by mass, C: 20 to 45% by mass, and O: 0.1 to 20.0% by mass. It is related with the said inorganic fiber for fiber bundles characterized by including.
- the present invention has a density of 2.7 g / cm 3 or more, a tensile strength of 2 GPa or more, and an elastic modulus of 250 GPa or more, Si: 50 to 70% by mass, C: 28 to 45% by mass, Al: 0.3%.
- the present invention relates to the inorganic fiber for a fiber bundle, characterized in that it is a crystalline silicon carbide fiber containing 06 to 3.8% by mass and B: 0.06 to 0.5% by mass and having a sintered structure of SiC.
- the present invention also provides a fiber bundle constituting an inorganic fiber bundle for a composite material in which an organosilicon polymer is spun, the obtained spun fiber is infusible, and the obtained infusible fiber is fired in an inert atmosphere.
- the firing treatment is performed without applying tension to the infusible fiber, and relates to a method for manufacturing an inorganic fiber for fiber bundles.
- the present invention also provides amorphous silicon carbide fibers containing 0.05 to 3% by mass of Al, 0.05 to 0.4% by mass of B, and 1 to 3% by mass of surplus carbon.
- the firing treatment is performed by applying tension to the amorphous silicon carbide fiber. It is related with the manufacturing method of the inorganic fiber for fiber bundles characterized by performing without applying.
- the present invention also relates to an inorganic fiber bundle for composite materials composed of the inorganic fiber for fiber bundle.
- the present invention also relates to a ceramic matrix composite material characterized in that the inorganic fiber bundle for composite materials is a reinforcing fiber and ceramics is a matrix.
- the present invention relates to the ceramic matrix composite material, wherein the inorganic fiber bundle for composite material is a two-dimensional or three-dimensional fabric, a unidirectional sheet, or a laminate thereof.
- the inorganic fiber bundle for composite materials composed of inorganic fibers for fiber bundles according to the present invention avoids contact between fibers without damaging the fibers in the inorganic fiber bundle, and an interfacial layer on the entire surface of each fiber
- a ceramic matrix composite material exhibiting sufficient strength and fracture energy and excellent durability when subjected to stress in a high temperature / oxidizing atmosphere. Obtainable.
- Example 1 Optical microscope photograph showing meandering pitch and meandering width of inorganic fiber for fiber bundle according to the present invention External view of drooping fiber in Example 1 External view of fired fiber in Example 1 (A) Example 1, (b) Example 2, (c) Comparative Example 1, (d) Example 3, (e) Comparative Example 2, (f) Example 4, (g) Comparative Example 3 Optical micrograph of the cross section of each fiber bundle
- the inorganic fiber for a fiber bundle according to the present invention is preferably a silicon carbide fiber in view of heat resistance and oxidation resistance.
- the inorganic fiber for fiber bundle according to the present invention meanders in the longitudinal direction, the meandering pitch is 3 to 40 mm, preferably 5 to 15 mm, and the meandering width is 0.1 to 5 mm, preferably 0.2 to 2 mm.
- the meandering pitch is less than 3 mm, the deviation of orientation due to meandering of each fiber increases with respect to the orientation direction of the fiber bundle in the composite material, and the fiber strength does not act effectively, thereby reducing the mechanical properties of the composite material. It is not preferable.
- the meandering pitch is larger than 40 mm, the space due to meandering becomes insufficient, and contact between fibers in the fiber bundle increases, which is not preferable.
- the meandering width is less than 0.1 mm, the space due to meandering becomes insufficient, and the contact between the fibers in the fiber bundle increases, which is not preferable.
- the meandering width is larger than 5 mm, the deviation of orientation due to meandering of each fiber increases with respect to the orientation direction of the fiber bundle in the composite material, the fiber strength does not act effectively, and the mechanical properties of the composite material are deteriorated. Therefore, it is not preferable.
- the meandering in the longitudinal direction means a state in which the fibers extend while meandering, and the meandering pitch is adjacent to each other among peaks and troughs repeated in the extending direction.
- the meandering width is the distance between the peaks of a mountain and a valley or the peak of a valley and a valley. It is called the distance in the vertical direction (width direction).
- this meandering pitch is obtained by continuously photographing a single fiber in the longitudinal direction with an optical microscope, and measuring the distance in the extension direction between an arbitrary peak and the apex of an adjacent valley from the optical microscope photograph. It can be determined by measuring and doubling the 10 average values.
- the meandering width can be obtained from an average value of 10 measured distances in the width direction between an arbitrary peak and the apex of the adjacent valley from an optical microscope.
- the inorganic fiber for fiber bundle according to the present invention has an element composition of Si: 45 to 60% by mass, Ti or Zr: 0.2 to 5% by mass, C: 20 to 45% by mass, O: 0.1 to 20 It is preferable to contain 0.0 mass%.
- Ti or Zr the heat resistance is improved, and in particular by adding Zr, the oxidation resistance and alkalinity can also be improved.
- the inorganic fiber bundle for composite material composed of the inorganic fiber for fiber bundle as a reinforcing fiber a ceramic matrix composite material having excellent characteristics can be obtained.
- the inorganic fiber for a fiber bundle according to the present invention has a density of 2.7 g / cm 3 or more, a tensile strength of 2 GPa or more, and an elastic modulus of 250 GPa or more, Si: 50 to 70% by mass, C: 28 to 45 % By mass, Al: 0.06 to 3.8% by mass, preferably 0.13 to 1.25% by mass, and B: 0.06 to 0.5% by mass, preferably 0.06 to 0.19% by mass It is preferable that it is a crystalline silicon carbide fiber containing a sintered structure of SiC. When the proportion of aluminum is excessively small, the alkali resistance of the crystalline silicon carbide fiber is lowered, and when the proportion is excessively high, mechanical properties at high temperatures are lowered.
- Crystalline silicon carbide fibers exhibiting excellent alkali resistance due to the excellent heat resistance and high strength and elastic modulus obtained by making it crystalline, and also the presence of aluminum are obtained, and are composed of inorganic fibers for this fiber bundle.
- the inorganic fiber bundle for composite material By using the inorganic fiber bundle for composite material as a reinforcing fiber, a ceramic matrix composite material having excellent characteristics can be obtained.
- the method for producing an inorganic fiber for a fiber bundle according to the present invention includes a spinning step of spinning an organosilicon polymer, and an infusibilization step of insolubilizing the obtained spun fiber by heat treatment in an oxidizing atmosphere or electron beam irradiation. And a firing step of firing the obtained infusible fiber in an inert atmosphere or a reducing atmosphere.
- the spinning process first comprises a carbosilane (—Si—CH 2 —) bond unit and a polysilane (—Si—Si—) bond unit, and has a hydrogen atom, lower alkyl group, aryl group, phenyl group on the side chain of silicon.
- an organosilicon polymer having a group selected from the group consisting of silyl groups, and heating a compound selected from the group consisting of an alkoxide of Ti or Zr, an acetylacetoxy compound, a carbonyl compound, a cyclopentadienyl compound, and an amine compound
- a Ti or Zr-containing organosilicon polymer is prepared by reaction. Next, this Ti or Zr-containing organosilicon polymer is melt-spun.
- the infusibilization step is performed, for example, by infusibilizing the obtained spun fiber.
- infusibility a method known per se can be adopted, the infusibilization temperature in an oxidizing atmosphere is 50 to 300 ° C., and the electron beam irradiation is 2 to 15 MVy / sec at an acceleration voltage of 2 to 4 MV. dose, 10-20 MGydose.
- the firing step is performed on the obtained infusible fiber in an inert atmosphere, preferably in the range of 1100 to 1600 ° C. without applying tension to the fiber.
- the fibers can be meandered in the longitudinal direction.
- the fiber shrinks in the radial direction and the longitudinal direction of the fiber in order to reduce the weight. It is to be.
- a fiber can meander in a longitudinal direction in the process in which an infusible fiber mineralizes.
- spinning is performed by a cans method, and a predetermined length (usually 500 to 1000 m) is spun into a circular shape with a diameter of 20 to 50 cm on a tray, and this is oxidized.
- Infusibilization is performed by heat treatment in a neutral atmosphere or electron beam irradiation. Next, this is achieved by firing in an inert atmosphere using a batch-type firing furnace or a pusher-type firing furnace capable of continuously firing a plurality of trays on which infusibilized fibers are set.
- the spinning is continuously wound around a drum, and then a predetermined length (usually 500 to 1000 m) is suspended in a circular shape having a diameter of 20 to 50 cm on a tray and then infusibilized.
- a predetermined length usually 500 to 1000 m
- it may be fired in an inert atmosphere using a batch-type firing furnace or a pusher-type firing furnace capable of continuously firing a plurality of trays in which infusible fibers are set. Good.
- Spinning fibers or infusible fibers have low strength, and the fibers may break during the drooping process. Therefore, after spinning by drum and continuously infiltrating, the fiber strength is increased without proceeding mineralization by continuous firing at 500-800 ° C in an inert atmosphere. Take it up on the bobbin. After that, a predetermined length (usually 500 to 1000 m) is hung in a circular shape with a diameter of 20 to 50 cm on the tray, and then a batch-type firing furnace or a plurality of trays with fibers set are continuously formed as described above. It may be fired in an inert atmosphere using a pusher type firing furnace that can be fired automatically.
- the continuous firing temperature is less than 500 ° C., there is no effect of increasing the fiber strength, and only the number of steps is increased, which is not preferable.
- the temperature is higher than 800 ° C., mineralization proceeds during firing, and subsequent weight reduction and volume shrinkage during firing become insufficient, the meander pitch becomes larger than 40 mm, and the meander width becomes less than 0.1 mm. Therefore, it is not preferable.
- the inorganic fiber for a fiber bundle according to the present invention can be practically used as an inorganic fiber bundle for a composite material after being fired in an inert atmosphere and wound around a bobbin. At this time, in order to improve the handleability of the fiber bundle, it is preferable to immerse in water, an organic solvent or a mixture of both in which a resinous sizing agent is dissolved and wind it while drying.
- the resinous sizing agent all known resins can be used. Specific examples thereof include poval resin, polyethylene oxide, epoxy resin, modified epoxy resin, polyester resin, polyimide resin, phenol resin, polyurethane resin. , Polyamide resin, polycarbonate resin, silicon resin, phenoxy resin, polyphenylene sulfide, fluorine resin, hydrocarbon resin, halogen-containing resin, acrylic acid resin, and ABS resin.
- poval resin and polyethylene oxide are used for commercially available inorganic fibers, and are particularly preferable.
- the amount of adhesion is not particularly limited, but is preferably 0.01 to 10% by mass, and particularly preferably 0.1 to 5% by mass with respect to the inorganic fiber. If it is less than 0.01% by mass, the fiber bundle does not converge, and if it exceeds 10% by mass, the degree of convergence does not change and the sizing agent is used wastefully.
- the fiber bundles After firing in a batch-type firing furnace or a pusher-type firing furnace that can continuously fire a plurality of trays in which infusibilized fibers are set, the fiber bundles are spun in the Kens form or suspended Since the circular shape remains, it is continuously fired in an inert atmosphere at 1100-1500 ° C. so that tension is not applied as much as possible, while maintaining the meandering pitch and meandering width, You may rewind.
- the inorganic fiber for fiber bundle according to the present invention is a crystalline silicon carbide fiber having a sintered structure of SiC
- the inorganic fiber for fiber bundle has 0.05 to 3% by mass of Al and 0% of B.
- Amorphous silicon carbide fiber containing 0.05 to 0.4 mass% and 1 to 3 mass% of excess carbon is fired without applying tension in a temperature and in an inert atmosphere within a range of 1600 to 2100 ° C. It can be obtained by processing and crystallizing.
- the process of crystallizing amorphous silicon carbide fiber during heating causes weight loss and shrinkage in the radial and longitudinal directions of the fiber, accompanied by volume shrinkage. It is to avoid restraint.
- the amorphous silicon carbide fiber which has the said meandering pitch and meandering width can be provided.
- the amorphous silicon carbide fiber preferably contains 8 to 16% by mass of oxygen. When heating the amorphous silicon carbide fiber, this oxygen desorbs the above-mentioned excess carbon as CO gas, and brings the ratio of Si and C close to the stoichiometric ratio of SiC, so that the crystalline silicon carbide fiber Can be obtained.
- the amorphous silicon carbide fiber is suspended in a circular shape having a predetermined length (usually 500 to 1000 m) and a diameter of 20 to 50 cm on a tray.
- firing is performed in an inert atmosphere at 1600 to 2100 ° C. It is achieved by making it.
- the bobbin can be wound up and used as a composite inorganic fiber bundle according to the present invention.
- This amorphous silicon carbide fiber can be prepared, for example, by the following method.
- the number average molecular weight of polysilane is usually 300 to 1000.
- the polysilane is obtained by heating the chain or cyclic polysilane to a temperature in the range of 400 to 700 ° C., or by adding a phenyl group-containing polyborosiloxane to the chain or cyclic polysilane.
- the polysilane partially having a carbosilane bond obtained by heating to a temperature in the range of 250 to 500 ° C.
- the polysilane can have a hydrogen atom, a lower alkyl group, an aryl group, a phenyl group or a silyl group as a side chain of silicon.
- a predetermined amount of aluminum alkoxide, acetylacetoxide compound, carbonyl compound, or cyclopentadienyl compound is added to polysilane, and 1 to 10 at a temperature usually in the range of 250 to 350 ° C. in an inert gas.
- an aluminum-containing organosilicon polymer that is a raw material for spinning is prepared.
- the amount of aluminum compound used is usually 0.14 to 0.86 mmol per gram of polysilane.
- An aluminum-containing organosilicon polymer is spun by a method known per se such as melt spinning or dry spinning to prepare a spun fiber.
- the spinning fiber is infusibilized in an oxidizing atmosphere to prepare an infusible fiber, which is then fired in an inert gas such as nitrogen or argon at a temperature in the range of 1100 to 1600 ° C.
- an inert gas such as nitrogen or argon at a temperature in the range of 1100 to 1600 ° C.
- a crystalline silicon carbide based fiber is prepared.
- the ceramic matrix composite material according to the present invention is characterized in that the inorganic fiber bundle for composite material obtained as described above is used as a reinforcing fiber, and ceramic is used as a matrix.
- the inorganic fiber bundle for composite materials Two-dimensional or three-dimensional textiles, such as a plain weave and a satin weave, a one-way sheet-like thing, or those laminated bodies may be sufficient.
- the volume ratio of the inorganic fibers in the composite material but 10 to 50% is common.
- the composite method is not particularly limited, but after coating a preform woven with inorganic fibers with boron nitride or carbon as an interface layer, a ceramic precursor polymer such as polycarbosilane, polymetallocarbohydrate, etc.
- a ceramic precursor polymer such as polycarbosilane, polymetallocarbohydrate, etc.
- a polymer impregnation / firing method in which silane, polysilazane, etc. are dissolved in a solvent such as xylene, impregnated and dried, and then heated and fired to form a composite, impregnated with a slurry of matrix raw material powder, and hot press etc.
- pressure-sintering method sol-gel method using matrix element alkoxide as raw material
- chemical vapor deposition method that forms matrix by reaction of reaction gas at high temperature
- a reaction sintering method can be used.
- the ceramic matrix of the present invention includes crystalline or amorphous oxide ceramics, crystalline or amorphous non-oxide ceramics, glass, crystallized glass, a mixture thereof, and those obtained by dispersing these ceramic particles. preferable.
- oxide ceramics include aluminum, magnesium, silicon, yttrium, indium, uranium, calcium, scandium, tantalum, niobium, neodymium, lanthanum, ruthenium, rhodium, beryllium, titanium, tin, strontium, barium, zinc, zirconium. And oxides of elements such as iron and complex oxides of these metals.
- non-oxide ceramics include carbides, nitrides and borides.
- carbide include carbides of elements such as silicon, titanium, zirconium, aluminum, uranium, tungsten, tantalum, hafnium, boron, iron, and manganese, and composite carbides of these elements.
- this composite carbide include inorganic substances obtained by heating and baking polytitanocarbosilane or polyzirconocarbosilane.
- nitrides include nitrides of elements such as silicon, boron, aluminum, magnesium, and molybdenum, composite oxides of these elements, and sialon.
- borides include borides of elements such as titanium, yttrium, and lanthanum, and platinum boride lanthanoids such as CeCoB 2 , CeCo 4 B 4 , and ErRh 4 B 4 .
- the glass include amorphous glass such as silicate glass, phosphate glass, and borate glass.
- crystallized glass include LiO 2 —Al 2 O 3 —MgO—SiO 2 glass and LiO 2 —Al 2 O 3 —MgO—SiO 2 —Nb 2 O 5 whose main crystal phase is ⁇ -spudene.
- the main crystal phase MgO-Al 2 O 3 -SiO 2 based glass is cordierite, the main crystal phase is barium male solid light BaO-MgO-Al 2 O 3 -SiO 2 based glass, the main crystalline phase Examples thereof include BaO—Al 2 O 3 —SiO 2 based glass that is mullite or hexacelsian, and CaO—Al 2 O 3 —SiO 2 based glass whose main crystal phase is anorthite.
- the crystal phase of these crystallized glasses may contain cristobalite.
- the ceramic in the present invention include solid solutions of the above-mentioned various ceramics.
- the ceramic matrix is selected from silicon nitride, silicon carbide, zirconium oxide, magnesium oxide, potassium titanate, magnesium borate, zinc oxide, titanium boride and mullite.
- examples include inorganic particles of spherical particles, polyhedral particles, plate-like particles, rod-like particles, and ceramics in which 0.1 to 60% by volume of whiskers are uniformly dispersed.
- the particle size of spherical particles and polyhedral particles is 0.1 ⁇ m to 1 mm, and the aspect ratio of plate-like particles, rod-like particles and whiskers is generally 1.5 to 1000.
- Example 1 0.5 parts by mass of polyborodiphenylsiloxane was added to 100 parts by mass of polydimethylsilane, and this mixture was heated and reacted at 380 ° C. for 10 hours in a nitrogen atmosphere to synthesize about 70 parts by mass of polycarbosilane having a weight average molecular weight of 1000. . 5 parts by mass of zirconium acetylacetonate was added to this polycarbosilane, and the mixture was reacted by heating at 300 ° C. for 3 hours in a nitrogen atmosphere to obtain polyzirconocarbosilane. The polyzirconocarbosilane was melt-spun while being continuously wound around a drum at about 250 ° C.
- FIG. 2 shows the appearance of the suspended fiber. Ten sets of these were produced and fired continuously at 1450 ° C. in nitrogen at a feed rate of 1 m / hour using a pusher-type firing furnace.
- FIG. 3 shows the appearance after firing.
- the obtained inorganic fiber bundle for composite material has a silicon carbide-based chemical composition having a mass ratio of Si: 55.5%, O: 9.8%, C: 34.1%, Zr: 0.6%. It was a fiber (average diameter: 12.5 ⁇ m, 800 pieces / fiber bundle, sizing agent: polyethylene oxide).
- the results of measuring the meander pitch and meander width are shown in Table 1. In the measurement, one fiber was continuously photographed in the longitudinal direction with an optical microscope, and the meandering pitch and meandering width at two arbitrary positions were measured from the photograph, and obtained from the average value of ten.
- the cross section in the inorganic fiber bundle for composite materials thus obtained was observed with an optical microscope.
- the micrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Example 2 An inorganic fiber bundle for a composite material was produced in the same manner as in Example 1 except that continuous baking after infusibilization in Example 1 was performed at 750 ° C. in a nitrogen atmosphere.
- the obtained inorganic fiber bundle for composite material has a silicon carbide-based chemical composition having a mass ratio of Si: 55.5%, O: 9.8%, C: 34.1%, Zr: 0.6%. It was a fiber (average diameter: 12.1 ⁇ m, 800 fibers / fiber bundle, sizing agent: polyethylene oxide). The results of measuring the meander pitch and meander width are shown in Table 1.
- the cross section in the inorganic fiber bundle for composite materials thus obtained was observed with an optical microscope.
- the micrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Comparative Example 1 The infusible fiber bundle obtained during the production of Example 1 was immersed in an aqueous solution containing 1% by mass of polyethylene oxide at 200 ° C. while continuously firing by applying a tension of 200 g at 1450 ° C. in a nitrogen atmosphere. It was wound up on a bobbin while being dried with a to prepare an inorganic fiber bundle for composite materials.
- the obtained inorganic fiber bundle for composite material has a silicon carbide-based chemical composition having a mass ratio of Si: 55.5%, O: 9.8%, C: 34.1%, Zr: 0.6%. It was a fiber (average diameter: 11 ⁇ m, 800 fibers / fiber bundle, sizing agent: polyethylene oxide). The meandering pitch and meandering width were unmeasurable because the fiber was running straight (described in Table 1).
- the cross section in the inorganic fiber bundle for composite materials thus obtained was observed with an optical microscope.
- the photomicrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Example 3 0.5 parts by mass of polyborodiphenylsiloxane was added to 100 parts by mass of polydimethylsilane, and this mixture was heated and reacted at 380 ° C. for 10 hours in a nitrogen atmosphere to synthesize about 70 parts by mass of polycarbosilane having a weight average molecular weight of 1000. . 10 parts by mass of tetrabutyl titanate was added to this polycarbosilane, and the mixture was reacted by heating at 300 ° C. for 3 hours in a nitrogen atmosphere to obtain polytitanocarbosilane.
- This polytitanocarbosilane was melt spun into a circular shape with a diameter of about 40 cm on a carbon tray by 800 kens method at about 250 ° C. with 800 multi-hole nozzles.
- infusibilization was performed by heat treatment in air at 180 ° C. for 5 hours. Then, it set in the state put on the tray in the batch-type baking furnace, and baked at 1400 degreeC in nitrogen for 1 hour. Then, it was immersed in an aqueous solution added with 1% by mass of polyethylene oxide, wound on a bobbin while being dried at 200 ° C., and an inorganic fiber bundle for a composite material composed of inorganic fibers for a fiber bundle meandering in the longitudinal direction was produced.
- the obtained inorganic fiber bundle for composite materials has a silicon carbide-based chemical composition with a mass ratio of Si: 54.4%, O: 10.2%, C: 33.9%, Ti: 1.5%. It was a fiber (average diameter: 12.5 ⁇ m, 800 pieces / fiber bundle, sizing agent: polyethylene oxide). The results of measuring the meander pitch and meander width are shown in Table 1.
- the cross section in the inorganic fiber bundle for composite materials thus obtained was observed with an optical microscope.
- the micrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Comparative Example 2 Polycarbosilane was prepared in the same manner as in Example 3, and melt spinning was performed while continuously winding on a drum instead of melt spinning on a tray by a melt spinning method. Then, after infusibilizing by heat treatment at 180 ° C. for 5 hours in air, it was immersed in an aqueous solution to which 1% by mass of polyethylene oxide was added while performing continuous firing with a tension of 100 g at 1400 ° C. in a nitrogen atmosphere. The fiber was wound around a bobbin while being dried at 200 ° C. to produce an inorganic fiber bundle for composite materials.
- the obtained inorganic fiber bundle for composite materials has a silicon carbide-based chemical composition with a mass ratio of Si: 54.4%, O: 10.2%, C: 33.9%, Ti: 1.5%. It was a fiber (average diameter: 11.3 ⁇ m, 800 fibers / fiber bundle, sizing agent: polyethylene oxide). The results of measuring the meander pitch and meander width are shown in Table 1.
- the cross section in the inorganic fiber bundle for composite materials thus obtained was observed with an optical microscope.
- the photomicrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Example 4 0.5 parts by mass of polyborodiphenylsiloxane was added to 100 parts by mass of polydimethylsilane, and this mixture was heated and reacted at 380 ° C. for 10 hours in a nitrogen atmosphere to synthesize about 70 parts by mass of polycarbosilane having a weight average molecular weight of 1000. . 4 parts by mass of aluminum trisecondary butoxide was added to this polycarbosilane, and the mixture was reacted by heating at 300 ° C. for 3 hours in a nitrogen atmosphere to obtain polyaluminocarbosilane. The polyaluminocarbosilane was melt-spun by continuously winding it on a drum at about 250 ° C.
- the results of measuring the meander pitch and meander width are shown in Table 1.
- the cross section in the inorganic fiber bundle for composite materials thus obtained was observed with an optical microscope.
- the micrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Comparative Example 3 The amorphous silicon carbide fiber containing 1.0% by mass of Al, 0.2% by mass of B, and 1.5% by mass of surplus carbon obtained during the production of Example 4 was subjected to tension. Crystallization with continuous heat treatment at 1800 ° C. in argon over 100 g, immersed in an aqueous solution added with 1% by mass of polyethylene oxide, wound on a bobbin while drying at 200 ° C., and an inorganic fiber bundle for composite materials Produced.
- the results of measuring the meander pitch and meander width are shown in Table 1.
- the cross section in the inorganic fiber bundle for composite material thus obtained was observed with an optical microscope.
- the micrograph is shown in FIG.
- the tensile strength of the obtained fiber bundle was measured by the JIS R7601 resin impregnated strand method, and the results are shown in Table 1.
- Examples 1, 2, 3, and 4 and Comparative Examples 1, 2, and 3 are described below. From FIG. 4, Examples 1, 2, 3, and 4 have a fiber bundle spread compared to Comparative Examples 1, 2, and 3, respectively. The effect of providing the meandering pitch and meandering width of the present invention in the direction is recognized. On the other hand, meandering in the longitudinal direction from Comparative Examples 2 and 3 has almost no effect outside the scope of the present invention, and is the same as the straight fiber of Comparative Example 1. Further, it can be seen that even if the meandering pitch and meandering width of the present invention are given in the longitudinal direction, the fiber strength is hardly affected. Thus, in the present invention, it can be seen that the fiber spacing in the fiber bundle can be increased widely and appropriately while maintaining the fiber strength.
- the interface layer had a thickness of about 0.5 ⁇ m at 1000 ° C. under reduced pressure using boron trichloride and ammonia as source gases and argon as a carrier gas.
- the matrix was densified at 1000 ° C. under reduced pressure using methyltrichlorosilane as a source gas and helium as a carrier gas. The porosity after forming the matrix was about 10%.
- a part of the three-dimensional fabric before complexing was loosened to extract a fiber bundle, and the tensile strength was measured by a JIS R7601 resin impregnated strand method. Moreover, the tensile test piece was processed from the produced ceramic matrix composite material, and the tensile strength and breaking strain at room temperature were measured. In addition, durability was evaluated by measuring the time to break by applying 60% of the tensile strength at room temperature at 1000 ° C. in the atmosphere. Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- Example 6 Using the inorganic fiber bundle for composite material of Example 2, a ceramic matrix composite material was produced in the same manner as in Example 5.
- Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- Example 7 Using the inorganic fiber bundle for composite material of Example 3, a ceramic matrix composite material was produced in the same manner as in Example 5.
- Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- Example 8 A ceramic matrix composite material was produced in the same manner as in Example 5 using the inorganic fiber bundle for composite material in Example 4.
- Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- Comparative Example 4 Using the inorganic fiber bundle for composite material of Comparative Example 1, a ceramic matrix composite material was prepared and evaluated in the same manner as in Example 5. Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- Comparative Example 5 Using the inorganic fiber bundle for composite material of Comparative Example 2, a ceramic matrix composite material was produced and evaluated in the same manner as in Example 7. Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- Comparative Example 6 Using the inorganic fiber bundle for composite material of Comparative Example 3, a ceramic matrix composite material was produced and evaluated in the same manner as in Example 8. Table 2 shows the tensile strength of the fiber extracted from the three-dimensional fabric, the tensile strength and breaking strain at room temperature of the ceramic matrix composite material, and 60% of the tensile strength at room temperature. Time to break at 1000 ° C. is shown.
- the ceramic matrix composite materials of Examples 5, 6, 7, and 8 both have slightly lower values in Example 6 in both tensile strength and fracture strain. These values are higher than those of Comparative Examples 4, 5, and 6, respectively. From the fracture surface observation, in Examples 5, 7, and 8, it was confirmed that there was no contact between the fibers in the fiber bundle, and the interface layer of boron nitride was uniformly formed on each fiber surface, and the fiber pull-out was also performed. Remarkably observed, it was confirmed that the interface layer was functioning effectively. This is considered to be the reason why high strength and fracture strain were obtained.
- Example 6 since the spread of the fiber bundle of Example 2 is smaller than the spread of the fiber bundle of Examples 1, 3, and 4, a part of the fiber bundle is compared with Examples 5, 7, and 8. Between the fibers was observed. At these contact points, the boron nitride interface layer is not formed, and the fiber pull-out is reduced, which is considered to be the reason for the slightly lower value.
- Example 6 With respect to the time to break at 1000 ° C. in the atmosphere with a stress of 60% of the tensile strength at room temperature of the ceramic matrix composite material, the ceramic matrix composite materials of Examples 5, 6, 7, and 8 are Although it is a slightly low value in Example 6, it shows a break time longer than Comparative Examples 4, 5, and 6, respectively.
- the pullout of the fiber was small compared to the fracture surface after the tensile test at room temperature, but it was observed remarkably, and the glass layer formation due to oxidation of the fiber and interface layer was slight. Met.
- Example 6 as compared with Examples 5, 7, and 8, a slightly larger number of glass layers were observed due to contact between fibers, which is considered to be a cause of a slightly lower value.
- the breaking time is the longest in Example 8 and the shortest in Example 7. This is because it depends on the heat resistance of the fiber itself, the heat resistance of the fiber of Example 4 is the best, and the heat resistance of the fiber of Example 3 is the poorest.
- the present invention can be used to manufacture inorganic fiber bundles for reinforcing fibers of ceramic matrix composite materials and ceramic matrix composite materials reinforced with these fibers.
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Abstract
Description
ポリジメチルシラン100質量部にポリボロジフェニルシロキサン0.5質量部を加え、この混合物を窒素雰囲気中、380℃で10時間加熱反応し、重量平均分子量1000のポリカルボシラン約70質量部を合成した。このポリカルボシランにジルコニウムアセチルアセトナートを5質量部添加し、窒素雰囲気中、300℃で3時間加熱反応し、ポリジルコノカルボシランを得た。このポリジルコノカルボシランを800個のマルチホールノズルにより、約250℃でドラムに連続に巻取りながら溶融紡糸を行った。ついで、空気中、180℃で5時間熱処理することにより不融化を行った。その後、窒素雰囲気中600℃で連続焼成を行い、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取った。ついで、カーボン製のトレイ上に直径約30cmの円形状に700m垂下した。図2に垂下した繊維の外観を示す。これを10組作製し、プッシャータイプの焼成炉を使用して、窒素中1450℃、送り速度1m/時間で連続的に焼成した。図3に焼成した後の外観を示す。無機化による重量減少と体積収縮により、全体に収縮していることがわかる。その後、ポリエチレンオキサイドを1質量%添加した水溶液にし、浸漬し200℃で乾燥させながらボビンに巻取り、長手方向に蛇行した繊維束用無機繊維から構成される複合材料用無機繊維束を作製した。
実施例1の不融化後の連続焼成を窒素雰囲気中750℃で行った以外は、実施例1と同じ方法で複合材料用無機繊維束を作製した。
実施例1の製造中に得られた、前記不融化した繊維束を、窒素雰囲気中1450℃で張力200gをかけて連続焼成を行いながら、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取り、複合材料用無機繊維束を作製した。
ポリジメチルシラン100質量部にポリボロジフェニルシロキサン0.5質量部を加え、この混合物を窒素雰囲気中、380℃で10時間加熱反応し、重量平均分子量1000のポリカルボシラン約70質量部を合成した。このポリカルボシランにテトラブチルチタネートを10質量部添加し、窒素雰囲気中、300℃で3時間加熱反応し、ポリチタノカルボシランを得た。このポリチタノカルボシランを800個のマルチホールノズルにより、約250℃でケンス方式によりカーボン製のトレイ上に直径約40cmの円形状に1000m溶融紡糸した。ついで、空気中、180℃で5時間熱処理することにより不融化を行った。その後、バッチ方式の焼成炉にトレイに乗せた状態でセットし、窒素中1400℃で1時間焼成した。その後、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取り、長手方向に蛇行した繊維束用無機繊維から構成される複合材料用無機繊維束を作製した。
実施例3と同様にポリカルボシランを準備し、溶融紡糸方法でトレイ上に溶融紡糸する代わりに、ドラムに連続に巻取りながら溶融紡糸を行った。その後、空気中、180℃で5時間熱処理することにより不融化を行った後、窒素雰囲気中1400℃で張力100gをかけて連続焼成を行いながら、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取り、複合材料用無機繊維束を作製した。
ポリジメチルシラン100質量部にポリボロジフェニルシロキサン0.5質量部を加え、この混合物を窒素雰囲気中、380℃で10時間加熱反応し、重量平均分子量1000のポリカルボシラン約70質量部を合成した。このポリカルボシランにアルミニウムトリセカンダリーブトキシドを4質量部添加し、窒素雰囲気中、300℃で3時間加熱反応し、ポリアルミノカルボシランを得た。このポリアルミノカルボシランを800個のマルチホールノズルにより、約250℃でドラムに連続に巻取りながら溶融紡糸を行った。ついで、空気中、180℃で5時間熱処理することにより不融化を行った。その後、窒素雰囲気中1400℃で連続焼成を行い、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取った。これにより、Alを1.0質量%、Bを0.2質量%、及び余剰の炭素を1.5質量%含有する非晶質炭化ケイ素系繊維を得た。ついで、カーボン製のトレイ上に直径約30cmの円形状に1000m垂下し、バッチ方式の焼成炉にトレイに乗せた状態でセットし、アルゴン中1800℃で1時間加熱処理し、結晶化させた。その後、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取り、長手方向に蛇行した繊維束用無機繊維から構成される複合材料用無機繊維束を作製した。
実施例4の製造中に得られた、Alを1.0質量%、Bを0.2質量%、及び余剰の炭素を1.5質量%含有する前記非晶質炭化ケイ素系繊維を、張力100gをかけてアルゴン中1800℃で連続的に加熱処理しながら結晶化させ、ポリエチレンオキサイドを1質量%添加した水溶液に浸漬し200℃で乾燥させながらボビンに巻取り、複合材料用無機繊維束を作製した。
実施例1の複合材料用無機繊維束を3次元織物(繊維割合は、X:Y:Z=1:1:0.2)に製織した。ついで、アルゴン中、1000℃でサイジング剤を分解除去後、化学気相蒸着法により窒化ホウ素の界面層、および炭化ケイ素のマトリックスを形成して、セラミックス基複合材料を作製した。界面層は、三塩化ホウ素とアンモニアを原料ガス、アルゴンをキャリアガスとして、減圧下、1000℃で約0.5μmの厚さとした。マトリックスはメチルトリクロロシランを原料ガス、ヘリウムをキャリアガスとして、減圧下、1000℃で緻密化を行った。マトリックス形成後の空隙率は約10%であった。
実施例2の複合材料用無機繊維束を用いて、実施例5と同じ方法で、セラミックス基複合材料を作製した。
実施例3の複合材料用無機繊維束を用いて、実施例5と同じ方法で、セラミックス基複合材料を作製した。
実施例4の複合材料用無機繊維束を用いて、実施例5と同じ方法で、セラミックス基複合材料を作製した。
比較例1の複合材料用無機繊維束を用いて、実施例5と同じ方法で、セラミックス基複合材料を作製し、評価を行った。表2に3次元織物から抽出した繊維の引張強度、作製したセラミックス基複合材料の室温での引張強度と破断ひずみ、及び、室温での引張強度の60%の応力をかけた状態で、大気中1000℃での破断までの時間を示す。
比較例2の複合材料用無機繊維束を用いて、実施例7と同じ方法で、セラミックス基複合材料を作製し、評価を行った。表2に3次元織物から抽出した繊維の引張強度、作製したセラミックス基複合材料の室温での引張強度と破断ひずみ、及び、室温での引張強度の60%の応力をかけた状態で、大気中1000℃での破断までの時間を示す。
比較例3の複合材料用無機繊維束を用いて、実施例8と同じ方法で、セラミックス基複合材料を作製し、評価を行った。表2に3次元織物から抽出した繊維の引張強度、作製したセラミックス基複合材料の室温での引張強度と破断ひずみ、及び、室温での引張強度の60%の応力をかけた状態で、大気中1000℃での破断までの時間を示す。
Claims (8)
- 複合材料用無機繊維束を構成する繊維束用無機繊維において、
長手方向に蛇行し、蛇行ピッチが3~40mmであり、蛇行巾が0.1~5mmであることを特徴する繊維束用無機繊維。 - 元素組成が、Si:45~60質量%、Ti又はZr:0.2~5質量%、C:20~45質量%、O:0.1~20.0質量%を含むことを特徴とする請求項1記載の繊維束用無機繊維。
- 密度が2.7g/cm3以上、引張強度が2GPa以上、弾性率が250GPa以上であり、Si:50~70質量%、C:28~45質量%、Al:0.06~3.8質量%及びB:0.06~0.5質量%を含み、SiCの焼結構造からなる結晶性炭化ケイ素繊維であることを特徴とする請求項1記載の繊維束用無機繊維。
- 有機ケイ素重合体を紡糸し、得られた紡糸繊維を不融化し、得られた不融化繊維を不活性雰囲気中で焼成する複合材料用無機繊維束を構成する繊維束用無機繊維の製造方法において、
前記焼成処理は、前記不融化繊維に張力を掛けずにおこなうことを特徴とする繊維束用無機繊維の製造方法。 - Alを0.05~3質量%、Bを0.05~0.4質量%、及び余剰の炭素を1~3質量%含有する非晶質炭化ケイ素系繊維を1600~2100℃の温度及び不活性雰囲気中で焼成し、結晶化させる複合材料用無機繊維束を構成する繊維束用無機繊維の製造方法において、
前記焼成処理は、前記非晶質炭化ケイ素系繊維に張力を掛けずにおこなうことを特徴とする繊維束用無機繊維の製造方法。 - 請求項1乃至3いずれか記載の繊維束用無機繊維から構成される複合材料用無機繊維束。
- 請求項6記載の複合材料用無機繊維束を強化繊維とし、セラミックスをマトリックスとすることを特徴とするセラミックス基複合材料。
- 複合材料用無機繊維束の形態が2次元若しくは3次元織物又は一方向シート状物、又はそれらの積層物であることを特徴とする請求項7記載のセラミックス基複合材料。
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- 2011-02-07 EP EP11756000.3A patent/EP2549001A4/en not_active Withdrawn
- 2011-02-07 JP JP2012505565A patent/JPWO2011114810A1/ja active Pending
- 2011-02-07 CN CN2011800142929A patent/CN102803589A/zh active Pending
- 2011-02-07 US US13/583,124 patent/US20130029127A1/en not_active Abandoned
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP2578556B1 (en) * | 2011-10-03 | 2017-06-28 | United Technologies Corporation | Method and ceramic component |
JP2017160066A (ja) * | 2016-03-07 | 2017-09-14 | 株式会社Ihiエアロスペース | 炭化ケイ素系複合体及びその製造方法 |
JP2018199604A (ja) * | 2017-05-29 | 2018-12-20 | イビデン株式会社 | SiC繊維強化セラミック複合材およびその製造方法 |
CN114380612A (zh) * | 2022-02-21 | 2022-04-22 | 江西信达航科新材料科技有限公司 | 低损耗高抗氧化碳化硅纤维增强氧化锆-钨酸锆陶瓷复合材料的制备方法 |
Also Published As
Publication number | Publication date |
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CN102803589A (zh) | 2012-11-28 |
JPWO2011114810A1 (ja) | 2013-06-27 |
EP2549001A4 (en) | 2013-10-30 |
US20130029127A1 (en) | 2013-01-31 |
EP2549001A1 (en) | 2013-01-23 |
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