WO2022118963A1 - セラミックス基複合材料とその製造方法 - Google Patents
セラミックス基複合材料とその製造方法 Download PDFInfo
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- WO2022118963A1 WO2022118963A1 PCT/JP2021/044514 JP2021044514W WO2022118963A1 WO 2022118963 A1 WO2022118963 A1 WO 2022118963A1 JP 2021044514 W JP2021044514 W JP 2021044514W WO 2022118963 A1 WO2022118963 A1 WO 2022118963A1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
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- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
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- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/667—Sintering using wave energy, e.g. microwave sintering
Definitions
- the present invention relates to a ceramic-based composite material and a method for producing the same.
- the ceramic-based composite material is a material in which ceramics such as silicon carbide are used as a matrix and reinforcing fibers are provided in the matrix. Ceramic-based composite materials are used as high-temperature structural members in rocket engines, aircraft jet engines, and the like.
- CVI Chemical Vapor Infiltration
- PIP Polymer Impregnation of Pyrolysis
- MI metal melt impregnation
- MI metal melt impregnation
- the fibrous body is also called a preform.
- the reactive gas is flowed through the heated fiber body, and the reactant of the reactive gas is deposited as a matrix in the pores inside the fiber body.
- a polymer such as polycarbosilane is impregnated into a fiber body, and the impregnated polymer is calcined to form a matrix.
- a matrix for example, a matrix of silicon carbide and metallic silicon
- a metal component for example, metallic silicon
- Patent Document 1 and Non-Patent Documents 1 and 2 describe techniques relating to a part of the embodiments of the present application.
- the above-mentioned PIP method, CVI method, and MI method each have problems.
- the PIP method and the CVI method it takes a long time to form a high-density matrix, which is a factor of cost increase.
- the MI method a high-density matrix can be formed in a relatively short time, but a metal remains, and the metal causes a decrease in heat resistance and oxidation resistance.
- Non-Patent Document 3 a combination technique of each method is proposed. For example, by combining the CVI method and the PIP method, and further the combination of the CVI method, the powder impregnation and the PIP method, the process period is shortened to 1/3.
- Patent Document 2 a film boiling method capable of forming a matrix at a speed 50 times or more faster than that of a single CVI process has been proposed (Patent Document 2 and Non-Patent Document 4). The conversion was insufficient.
- an object of the present invention focuses on maximizing the effect of the film boiling method, and provides a technique capable of forming a high-density matrix in a short time by using the film boiling method in a method for producing a ceramic-based composite material. To do.
- the production method according to the present invention is a method for producing a ceramic-based composite material including a matrix and reinforcing fibers provided in the matrix.
- A The fiber body composed of the reinforcing fibers is impregnated with the powder of the ceramic material to be a part of the matrix.
- B The fibrous body impregnated with the powder is placed in the liquid raw material of the matrix.
- C By heating the fiber body in this state, the liquid raw material is brought into a film boiling state, and ceramics derived from the liquid raw material are generated in the fiber body as a part of the matrix.
- the effect of the membrane boiling method is maximized by combining powder impregnation, and high density is realized in a short time.
- the membrane boiling method even if the porosity is the same, if the pore size is large, the matrix cannot be completely filled, and pores remain as a factor of density decrease.
- the matrix can be filled in a short time if the pores are small in size. Therefore, by impregnating the fiber body with the powder of the ceramic material in advance, the pore size is subdivided, and then a matrix is formed by the film boiling method to realize high density in a short time.
- FIG. 2B-2B arrow view of FIG. 2A It is a 2C-2C arrow view of FIG. 2A.
- An example of a configuration that can be used for carrying out the membrane boiling method of the production method according to the embodiment of the present invention is shown.
- It is an image by a scanning electron microscope of the cross section of the ceramic-based composite material obtained by the Example of this invention.
- FIG. 4 is an enlarged view of a portion surrounded by a broken line in FIG.
- FIG. 5 is an enlarged view of a portion surrounded by a broken line in FIG.
- the production method according to the embodiment of the present invention is a method for producing a ceramic-based composite material provided with reinforcing fibers (fibers formed of reinforcing fibers) and a matrix. By dispersing, it is a method of obtaining a high-speed and high-density matrix in the film boiling method.
- the ceramic-based composite material is a matrix in which a large number of reinforcing fibers are provided as reinforcing materials.
- the ceramic-based composite material may be used as a high-temperature structural member in a rocket engine, an aircraft jet engine, or the like.
- the matrix may be formed of ceramics.
- the matrix may be formed of silicon carbide, but may be formed of another material (eg, mullite).
- the reinforcing fiber may be a fiber containing silicon carbide or carbon as a main component.
- the reinforcing fiber is silicon carbide fiber or carbon fiber.
- the reinforcing fiber is not limited to these, and may be, for example, a heat-resistant oxide fiber such as an alumina fiber, a mullite fiber, or a zirconia fiber.
- the reinforcing fibers may be provided in the matrix as a fiber body formed by a large number of reinforcing fibers. This fibrous body may be a woven or knitted fabric of reinforcing fibers. Further, although the fiber body is partially formed with a matrix by the CVI method, the PIP method, or the like, a large number of pores may still remain.
- FIG. 1 is a flowchart showing a method for manufacturing a ceramic-based composite material according to an embodiment of the present invention.
- step S1 the above-mentioned fiber body formed of a large number of reinforcing fibers is impregnated with a powder of a ceramic material (hereinafter, also simply referred to as powder).
- This powder may be calcined, and in one example, it is a silicon carbide powder (SiC powder), but it may be a powder of another material as described later.
- the fiber body used in step S1 may be one in which a matrix is partially formed by the CVI method, the PIP method, or the like. In this case, a matrix may be partially formed inside and / or both of the inside and the surface of the fiber.
- Step S1 may have steps S11 to S13.
- the median diameter (particle diameter with a cumulative height of 50%) of the powder used in step S1 may be 1 ⁇ m or more and 20 ⁇ m or less.
- the powder used in step S1 may be, for example, a mixed powder of a powder having a median diameter of 5 ⁇ m and a powder having a median diameter of 17 ⁇ m.
- the particle size of the particles constituting the powder used in step S1 (the particle size of the particles of 70% or more, 80%, or 90% or more of the whole powder) may be 1 ⁇ m or more and 20 ⁇ m or less.
- the powder used in step S1 may be composed of particles having one kind of particle size or may be composed of particles having a plurality of types of particle size.
- the powder used in step S1 may mainly consist of particles having a particle size of about 5 ⁇ m (for example, 3 ⁇ m or more and 7 ⁇ m or less) (70% or more, 80%, or 90% or more of the whole powder). ..
- the powder used in step S1 mainly contains particles having a particle size of about 5 ⁇ m (for example, 3 ⁇ m or more and 7 ⁇ m or less) and a particle size of about 5 ⁇ m (for example, 3 ⁇ m or more and 7 ⁇ m or less).
- each of the particles having a particle size of about 5 ⁇ m and the particles having a particle size of about 17 ⁇ m may occupy 40% or more of the powder used in step S1.
- the particle size of each particle (the diameter of the particle) may mean the maximum dimension of the particle (the maximum value among the dimensions in each direction).
- step S11 a slurry is generated by mixing a ceramic material powder with a liquid (dispersion medium) such as water.
- step S12 the fibrous body is put into a slurry container (not shown) in which the slurry generated in step S11 is held inside. At this time, the entire fiber body is buried in the slurry.
- step S12 the inside of the slurry container is evacuated through an intake pipe connected to the slurry container (gas phase portion inside the container). This promotes the filling of the slurry into the pores in the fiber.
- step S13 the fiber body impregnated with the slurry in step S12 is taken out from the slurry container, the fiber body is heated by an appropriate heating device, and the liquid is evaporated from the slurry in the fiber body. This causes only the liquid to evaporate from the slurry. This keeps the powder inside the fiber.
- step S11 After step S13, the above-mentioned step S11 may be started again and steps S11 to S13 may be repeated. After repeating steps S11 to S13 a predetermined number of times, the process proceeds to step S2.
- the predetermined number of times may be 2 times or more and 10 times or less (for example, 5 times).
- the predetermined number of times is two times, and in the first step S13, the fibrous body is heated at 80 ° C. for 30 minutes, and in the second step S13, the fibrous body is heated at 130 ° C. for 30 to 60 minutes. It is not necessary to repeat steps S11 to S13. In this case, if steps S11 to S13 are performed once, the process proceeds to step S2.
- step S2 the fiber body (the fiber body in which the powder is held inside) impregnated with the powder of the ceramic material in step S1 is placed in the liquid raw material of the matrix.
- the liquid raw material used in step S2 is a ceramic raw material described later as a matrix of ceramic-based composite materials.
- This liquid raw material may be, for example, polycarbosilane (LPCS: Liquid Polycarbosilane), which is a liquid raw material for silicon carbide.
- LPCS Liquid Polycarbosilane
- the liquid raw material is not limited to this, as will be described later.
- step S2 the above-mentioned fiber body is attached to the heating body by a fixture, and the fiber body is arranged together with the heating body in the liquid raw material of the matrix.
- the fiber body may or may not be in contact with the heating body in a state where the fiber body is attached to the heating body by the attachment tool.
- Step S2 has step S21 and step S22.
- step S21 the above-mentioned fiber body is attached to the heating body by the attachment tool.
- the fibrous body and the heated body may be in a state of being integrated with each other.
- the number of fibrous bodies attached to the heated body in this way may be one or a plurality (two in the example of FIG. 2A described later).
- FIG. 2A shows an example of a fixture that can be used in step S21.
- the attachment is not limited to the configuration example of FIG. 2A, and may be any one that maintains the state in which the fiber body is attached to the heating body.
- FIG. 2A shows a state in which the two fiber bodies 10 after the treatment in step S1 are attached to the heating body 1 so as to be in contact with the upper surface and the lower surface of the heating body 1 by the attachment tool 20 (hereinafter, also simply referred to as an attachment state). Is shown.
- the fixture 20 includes a pair of heat insulating plates 2, a porous body 3, an action mechanism 4, a heat insulating material 5, and a hanging portion 7.
- the heating body 1 is made of a material (for example, graphite) that is induced to be heated, and is arranged between a pair of heat insulating plates 2.
- Each heat insulating plate 2 is made of a material having heat insulating performance (for example, alumina).
- Each heat insulating plate 2 and the heating body 1 may be circular, for example, having the same radius when viewed from the thickness direction of the heat insulating plate 2.
- the porous body 3 is arranged between the heating body 1 and each heat insulating plate 2 in the above-mentioned mounting state.
- Each porous body 3 has a large number of holes through which a fluid can pass, and may be, for example, a stack of a plurality of wire meshes.
- the mechanism of action 4 has a bolt 4a and a nut 4b.
- the bolt 4a penetrates the two heat insulating plates 2 and the heating body 1 with a gap, and nuts 4b are screwed to both ends of each bolt 4a.
- each porous body 3 In the mounted state, by tightening the nut 4b to the bolt 4a in the direction of bringing the two heat insulating plates 2 closer to each other, each porous body 3, the heating body 1 and each fiber body 10 are sandwiched between the pair of heat insulating plates 2. Is retained.
- a plurality of such action mechanisms 4 may be provided.
- the heat insulating material 5 covers the outer periphery of the heating body 1 and the two fiber bodies 10 in the attached state. That is, the heating body 1 and each fiber body 10 have outer circumferences 1a and 10a surrounding the central axis facing the thickness direction of the heat insulating plate 2, respectively, and these outer peripherals 1a and 10a are attached to the heat insulating material 5 as shown in FIG. 2B. Be covered. In FIG. 2A, only the portions of the heat insulating material 5 located on both sides (left and right sides in this figure) of the heating body 1 and each fiber body 10 are shown by a two-dot chain line.
- the heat insulating material 5 is made of a material having heat insulating performance.
- the heat insulating material 5 may be a glass heat insulating cloth (woven fabric).
- the heat insulating material 5 may be wound with a wire 6 from the outer peripheral side thereof in order to fix the heat insulating material 5 to the heating body 1, but by other means. , The heat insulating material 5 may be fixed.
- each porous body 3 is open to the outer peripheral side. That is, each porous body 3 has an outer peripheral portion 3a surrounding a central axis facing the thickness direction of the heat insulating plate 2, and the outer peripheral portion 3a is open to the outside in the radial direction with respect to the central axis.
- FIG. 2C is a 2C-2C arrow view of FIG. 2A.
- the hanging portion 7 has a plate-shaped member 7a and a rod-shaped member 7b.
- the plate-shaped member 7a extends elongated in the left-right direction of FIGS. 2A and 2C along the upper surface of the upper heat insulating plate 2.
- Bolts 4a penetrate through both ends of the plate-shaped member 7a with a gap. Both ends of the plate-shaped member 7a are sandwiched between the upper heat insulating plate 2 and the upper nut 4b, respectively.
- a connecting portion 7a1 is provided at the center of the plate-shaped member 7a.
- a rod-shaped member 7b is connected to the connecting portion 7a1.
- the rod-shaped member 7b extends upward from the joint portion 7a1.
- a protruding portion as a bolt on the upper surface of the joint portion 7a1
- a bolt hole is formed on the lower end surface of the rod-shaped member 7b, and the bolt and the bolt hole are screwed together.
- the coupling portion 7a1 and the rod-shaped member 7b may be coupled.
- step S22 the fiber body 10 attached to the heating body 1 by the fixture 20 is arranged in the liquid raw material 9 in the processing container 8.
- the fiber body 10 is arranged in the liquid raw material 9, and the fiber body 10 is prevented from contacting the inner surface (bottom surface and inner peripheral surface) of the processing container 8 with the fixture 20, the heating body 1, and the fiber body 10.
- the heating body 1 is suspended by the suspending portion 7.
- the rod-shaped member 7b of the hanging portion 7 is arranged so as to penetrate the through hole 8a1 of the lid member 8a that closes the opening on the upper surface of the processing container 8, and the upper end side portion of the rod-shaped member 7b is not shown. It may be attached to and supported by an object by an appropriate means.
- step S22 the hanging portion suspends the fiber body and the heating body so that the fixture, the heating body, and the fiber body do not come into contact with the inner surface of the processing container (that is, separate from the inner surface of the processing container).
- the configuration is not limited to the configuration examples shown in FIGS. 2A and 2C and the like.
- the processing container 8 is made of a non-conductive material (for example, glass) that is not induced and heated.
- the processing container 8 has a gas introduction hole 8b for introducing nitrogen gas into the gas phase portion in the processing container 8 at the time of step S3 described later, and a gas for discharging gas from the gas phase portion in the processing container 8 at the time of step S3.
- the discharge hole 8a2 may be formed.
- step S22 the entire fiber body is located in the liquid raw material.
- the liquid raw material enters (penetrates) into each pore (each pore opening to the outside of the fiber) in the fiber impregnated with the powder in step S1.
- the process proceeds to step S3.
- step S3 a ceramic-based composite material is obtained by forming a matrix with respect to the fibrous body by the film boiling method.
- Step S3 includes step S31 and step S32.
- step S31 by heating the reinforcing fiber until the temperature of the reinforcing fiber (fiber body) becomes equal to or higher than the target temperature on the high temperature side, ceramics derived from the liquid raw material are generated in the pores inside the fiber impregnated with the powder. Let me. As a result, a matrix in which the ceramics and the powder are integrated is generated.
- step S31 the liquid raw material is heated by the heated fiber body and the powder in the fiber body, so that the film boils at the interface between the fiber body or the powder (inner surface of the pores in the fiber body) and the liquid raw material. It becomes a gas (that is, a film boiling state), and the film boiling gas produces and deposits ceramics (that is, thermal decomposition precipitates as ceramics) in the pores.
- the ceramics may be produced by one or both of the following methods (i) and (ii).
- the ceramics may also precipitate at the interface between the outer surface of the fiber and the liquid raw material.
- the heating in step S31 may be performed by inducing heating the heated body.
- the heating element 1 is induced and heated by an alternating magnetic field generated by the coil 11 by passing an alternating current through the coil 11.
- the fibrous body and the liquid raw material are heated by the heat generated by the heated heated body.
- the process proceeds to step S32.
- the target temperature on the high temperature side is a temperature higher than the boiling point of the liquid raw material.
- the rate of temperature rise of the fibrous body (or heated body) in step S31 is preferably 3000 ° C / hour or less, 2000 ° C / hour or less, or 1500 ° C / hour or less.
- the heating rate may be 500 ° C./hour or higher.
- the temperature rising rate is more preferably about 1000 ° C./hour or 1000 ° C./hour or less.
- the heating rate is not limited to this.
- the rate of temperature rise may be lower than 500 ° C./hour (in this case, the rate of temperature rise may be, for example, 100 ° C./hour or higher).
- step S31 when the heated body is induced to be heated as described above, the processing container 8 made of the non-conductive material is not induced to be heated.
- the heating body 1, the fiber body 10, and the fixture 20 are suspended by the hanging portion 7 so as not to come into contact with the inner surface of the processing container 8, so that the processing container 8 is hung. It is prevented from being damaged by coming into contact with the high temperature heating body 1, the fiber body 10, and the fixture 20.
- step S32 the fiber is cooled to a target temperature lower than the boiling point of the liquid raw material. This stops the production of the above-mentioned membrane boiling gas. As a result, in a state where the boiling phenomenon is stopped and new film boiling gas is not generated, the already generated film boiling gas is replaced with the liquid raw material, so that the liquid raw material becomes ceramics (ceramics) in the fiber body. Re-enters (penetrates) each pore that is not completely filled with. For example, the liquid raw material re-enters (permeates) the pores partially filled with ceramics by step S32.
- the temperature lowering rate of the body) may be, for example, a rate of spontaneous cooling or a rate of active cooling, as described later.
- the cooling in step S32 may be natural cooling performed by stopping the heating of the fibrous body and maintaining this stopped state.
- the liquid raw material in addition to stopping the heating of the fiber body, the liquid raw material may be positively cooled.
- a part of the liquid raw material 9 in the processing container 8 is flowed to the outside of the processing container 8, the liquid raw material 9 is cooled by a heat exchanger, and then the cooled liquid raw material 9 is used in the processing container 8.
- the liquid raw material 9 may be circulated so as to return to the inside.
- a pipe or a pump (not shown) for circulating the liquid raw material 9 may be provided in this way.
- step S31 is started again.
- the temperature measured by the above-mentioned temperature sensor is set as the temperature of the fiber body, and when the measured temperature becomes equal to or lower than the target temperature, step S31 is started again.
- the target temperature may be an approximate standard. That is, since it may be difficult to start step S31 again at the timing when the target temperature is reached, the timing for starting step S31 again may be when the temperature of the fiber body reaches the target temperature. It may be when the temperature of the fiber body falls below the target temperature to some extent.
- step S31 is started.
- This confirmation may be made, for example, by visually recognizing a transparent glass processing container from the outside. Since no bubbles are generated, it can be determined that the liquid raw material has completely penetrated into the inside of the fiber body.
- step S31 is started again, and steps S31 and S32 are repeated.
- the number of ceramics generated in each pore in the matrix increases, and the ceramics are filled in these pores.
- Steps S31 and S32 are repeated until each pore is fully (eg, completely) filled with ceramics.
- the number of repetitions may be, for example, 10 times or more and 20 times or less, but is not limited thereto.
- the target temperature in step S31 performed in a later stage may be higher than the target temperature in step S31 performed in the previous stage.
- the target temperature in step S31 may be increased by a plurality of steps (for example, three or more steps) in the repetition.
- the target temperature is 1000 ° C. in step S31 of the first stage (for example, from the first time to the third time), and the target temperature is said to be the target temperature in step S31 of the intermediate stage (for example, from the fourth time to the sixth time). Is 1100 ° C., and the target temperature may be 1200 ° C. in step S31 of the final step (for example, from the 7th time to the 12th time).
- the above-mentioned ceramics are silicon carbide.
- the boiling point of LPCS rises from about 180 ° C. to about 250 ° C. as the polymerization progresses in the repeating process of steps S31 and S32.
- the maximum temperature of the fiber body reached by step S31 is, for example, 800 ° C. or higher, preferably 1000 ° C. or higher and 1400 ° C. or lower.
- the maximum temperature is 1000 ° C or higher, sufficient progress of mineralization of ceramics can be expected, and when the maximum temperature is 1400 ° C or lower, the precipitation rate of ceramics becomes too high and the ceramics are deposited. It is possible to prevent severe thermal decomposition from occurring to the extent that it does not occur. This can be expected to facilitate the filling of ceramics in the pores inside the fiber.
- Example 1 the fiber body is formed of SiC fiber (silicon carbide fiber) as a reinforcing fiber, and the liquid raw material is the above-mentioned LPCS. Further, the processing shown in the flowchart of FIG. 1 described above was performed using the configurations shown in FIGS. 2A to 2C and FIG.
- FIG. 4 is an image of a cross section of the ceramic-based composite material obtained in Example 1 by a scanning electron microscope.
- FIG. 5 is an enlarged view of a portion surrounded by a broken line in FIG.
- FIG. 6 is an enlarged view of a portion surrounded by a broken line in FIG.
- reference numeral P indicates the powder of the ceramic material used in the above-mentioned step S1
- reference numeral F indicates the ceramics formed by the film boiling method of the above-mentioned step S3.
- FIG. 7 is an image of a cross section of the ceramic-based composite material obtained by the reference example by a scanning electron microscope.
- the above-mentioned steps S2 and S3 were performed without performing the above-mentioned step S1.
- Other points of the reference example are the same as those of the first embodiment.
- the image of FIG. 7 is an image having the same magnification as that of FIG.
- the minute (several ⁇ m) pores of the powders P are filled with the ceramics F generated in the above step S31. Therefore, according to the present embodiment, it can be seen that a matrix composed of the powder P and the ceramics F is formed inside the fiber body with a high filling rate.
- Example 2 In Example 2, the particle size of the ceramic material powder used in step S1 was changed to a plurality of values, and the process shown in the flowchart shown in FIG. 1 was performed.
- FIG. 8 is a table showing the results of Example 2.
- FIG. 8 (1) shows the case of a reference example in which the above-mentioned steps S2 and S3 are performed without performing the above-mentioned step S1. Other points of the reference example are the same as those of the second embodiment.
- (2) to (7) show the case of the second embodiment.
- (3) and (4) show the case of the ceramic-based composite material obtained simultaneously on the lower side and the upper side of the heating body 1 in FIG. 3, respectively, and (5) and (6) are shown in FIG. 3, respectively. The case of the ceramic-based composite material obtained simultaneously on the lower side and the upper side of the heating body 1 is shown.
- the “powder particle size” indicates the particle size of the particles constituting the powder used in step S1, and is described here as the particle size (median diameter) having a cumulative height of 50%.
- (7) shows a case where a mixed powder of a powder composed of particles having a particle size of 5.5 ⁇ m and a powder composed of particles having a particle size of 17.0 ⁇ m is used as the powder of step S1. ..
- the “treatment condition” indicates how many times the fiber body is heated to each temperature in the repetition of the above-mentioned steps S31 and S32.
- the fibrous body is heated to 1000 ° C. in the first step S31 from the first step to the third step, the fibrous body is heated to 1100 ° C. in the step S31 from the fourth step to the sixth step, and the fibrous body is heated to 1100 ° C. from the seventh step to the 12th step. It is shown that the fiber body was heated to 1200 ° C. in step S31 up to the second time.
- the “density after FB treatment” indicates the density of the ceramic-based composite material produced after the treatment of FIG. 1, and the “density increase amount” is the density of the ceramic-based composite material with respect to the density of the fibrous body.
- the “powder effect” indicates the ratio of the density increase amount in each case to the case where the density increase amount in the case of (1) is 1.
- the density is increased in each of the cases (2) to (7) in which the fiber is impregnated with the powder, as compared with the case of (1) in which the fiber is not impregnated with the powder.
- the "powder effect" was the highest in the case of (2) having a particle size of 5.5 ⁇ m. ..
- the “powder effect” was higher than that in the case of (2). That is, the maximum powder effect was obtained by using a mixed powder of a powder having a particle size of about 5 ⁇ m and a powder having a particle size of about 17.0 ⁇ m.
- the powder used in step S1 described above is a silicon carbide powder, but may be a powder of another ceramic material.
- the powder may be a powder of boron nitride (BN), which is a ceramic.
- Boron nitride has low adhesion to silicon carbide. Therefore, when the ceramics produced from the liquid raw material in step S31 described above are silicon carbide, or when the reinforcing fibers are silicon carbide fibers, at the interface between the boron nitride portion and the silicon carbide portion in the matrix. , The propagation of cracks can be suppressed.
- the powder may be carbon powder.
- the carbon powder has a function of suppressing the propagation of cracks as in the case of the above-mentioned boron nitride powder.
- the powder may be a powder of silicon dioxide (SiO 2 ) or alumina (Al 2 O 3 ), which is cheaper than silicon carbide.
- the powder may be a powder of mullite (Al 2 O 3 -SiO 2 ), which has higher heat resistance than alumina and is cheaper than silicon carbide.
- the powder may be a zirconia (ZrO 2 ) powder. Since zirconia is a ceramic having a higher melting point than silicon carbide, it does not melt and functions as a part of the matrix even in an ultra-high temperature environment.
- zirconia is a ceramic having a higher melting point than silicon carbide, it does not melt and functions as a part of the matrix even in an ultra-high temperature environment.
- the powder may be zirconium carbide (ZrC), hafnium (HfO 2 ), hafnium carbide (HfC), zirconium boride (ZrB 2 ), or hafnium boride (HfB 2 ) powder. These powders have the same function as zirconia powders.
- the powder may be a mixed powder of alumina powder and manganese oxide (MnO) powder.
- MnO manganese oxide
- oxygen enters the cracks generated in the matrix it reacts with silicon carbide in the matrix (silicon carbide produced as ceramics by the film boiling method in step S3) to generate silicon dioxide.
- silicon dioxide reacts with alumina to fill the cracks.
- Manganese oxide also activates the filling of such cracks.
- the liquid raw material used in step S3 described above may be a liquid raw material other than the LPCS described above.
- the liquid raw material may be boradin, methyltrichlorosilane, cyclohexane, silicon alkoxide solution, aluminum alkoxide solution, a mixed solution of silicon alkoxide solution and aluminum alkoxide solution, or a zirconium alkoxide solution.
- the ceramics produced by the heating in step S31 described above are boron nitride (BN), which is a ceramic.
- BN boron nitride
- the function of this boron nitride is the same as that described in the first modification.
- the ceramics produced by the heating in step S31 described above are silicon carbide (SiC), which is a ceramic, as in the case where the liquid raw material is polycarbosilane (LPCS).
- the ceramics produced by the heating in step S31 described above are carbon. This carbon has the same function as in the case of boron nitride.
- the ceramics produced by the heating in step S31 described above are silicon dioxide. Silicon alkoxide solutions are cheaper than LPCS.
- the ceramics produced by the heating in step S31 described above are alumina.
- Aluminum alkoxide solutions are cheaper than LPCS.
- the ceramics produced by the heating in step S31 described above are mullite.
- the ceramics produced by the heating in step S31 described above are zirconia.
- the function of this zirconia is the same as that described in the first modification.
- the liquid raw material used in step S3 is not limited to the above-mentioned specific example, and may be another liquid raw material.
- another metal alkoxide solution may be used as the liquid raw material used in step S3.
- the ceramics produced by the heating in step 31 described above may be oxide ceramics.
- the liquid raw materials used in step S3 are, for example, three as described in Non-Patent Document 1 so that the ceramics produced in step S31 are barium aluminosilicate (BaAl 2 Si 2 O 8 ). It may be a mixed solution of an alkoxide solution (alkoxydes).
- the liquid raw material used in step S3 is a mixed solution of a plurality of alkoxide solutions (alkoxydes) as described in Non-Patent Document 2 above. It may be there.
- step S31 may be performed without performing step S32.
- the fiber is heated until the temperature of the fiber becomes equal to or higher than the target temperature on the high temperature side, and the temperature of the fiber is kept above the target temperature for a predetermined time.
- This predetermined time may be, for example, 6 hours or more and 20 hours or less.
- the heating body 1 is omitted, and in step S31, a fiber body impregnated with powder (for example, a fiber body formed of carbon fiber or silicon carbide fiber) having a sufficiently large heat capacity (volume) is induced and heated.
- powder for example, a fiber body formed of carbon fiber or silicon carbide fiber
- the above-mentioned film boiling gas may be generated, and ceramics may be deposited in the pores of the matrix of the ceramic-based composite material by one or both of the above (i) and (ii).
- the heating body 1 is omitted, the number of ceramic-based composite materials 10 becomes one, and one ceramic-based composite material 10 comes into contact with the porous body 3 from above and below.
- the heat insulating material 5 may cover the outer periphery 10a of the ceramic-based composite material 10 and may be the same as described above in other respects. Further, the heat insulating plate 2 may be omitted in addition to the omission of the heating body 1 or instead of the omission of the heating body 1.
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Abstract
Description
(A)強化繊維により構成された繊維体に、前記マトリックスの一部となるセラミックス材料の粉末を含浸させ、
(B)前記粉末が含浸させられた前記繊維体を前記マトリックスの液体原料内に配置し、
(C)この状態で前記繊維体を加熱することにより、前記液体原料を膜沸騰状態にして、前記液体原料に由来するセラミックスを前記マトリックスの一部として前記繊維体内に生じさせる。
あるいは、ステップS1で用いる粉末を構成する粒子の粒径(粉末全体の70%以上、80%、又は90%以上の粒子の粒径)は、1μm以上であって20μm以下であってよい。また、ステップS1で用いる粉末は、1種類の粒径の粒子からなるものであってもよいし、複数種類の粒径の粒子からなるものであってもよい。前者の場合、ステップS1で用いる粉末は、主に(粉末全体の70%以上、80%、又は90%以上が)、粒径が5μm程度(例えば3μm以上7μm以下)の粒子からなっていてよい。後者の場合、ステップS1で用いる粉末は、主に(粉末全体の70%以上、80%、又は90%以上が)、粒径が5μm程度(例えば3μm以上7μm以下)の粒子と、粒径が17μm程度(15μm以上19μm以下)の粒子とからなっていてよい。また、後者の場合、粒径が5μm程度の粒子と、粒径が17μm程度の粒子の各々は、ステップS1で用いる粉末の40%以上を占めていてよい。
なお、各粒子の粒径(さしわたし)は、当該粒子の最大寸法(各方向の寸法のうちの最大値)を意味してよい。
本実施形態の実施例1では、繊維体を、強化繊維としてのSiC繊維(炭化ケイ素繊維)で形成されたものとし、液体原料を上述のLPCSとした。また、図2A~図2Cと図3に示す構成を用いて、上述の図1のフローチャートに示す処理を行った。
実施例2では、ステップS1で用いるセラミックス材料の粉末の粒径を複数の値に変えて、図1に示すフローチャートに示す処理を行った。図8は、実施例2の結果を示す表である。
上述のステップS1で用いた粉末は、炭化ケイ素の粉末であったが他のセラミックス材料の粉末であってもよい。
上述のステップS3において、ステップS32を行わずに、ステップS31を行ってもよい。この場合、ステップS31において、繊維体の温度が高温側の目標温度以上になるまで、繊維体を加熱し、所定時間、繊維体の温度を当該目標温度以上に保つ。この所定時間は、例えば、6時間以上20時間以内であってよい。
上述において、加熱体1を省略して、ステップS31では、熱容量(体積)が十分に大きい、粉末が含浸させられた繊維体(例えば炭素繊維又は炭化ケイ素繊維により形成された繊維体)を誘導加熱することにより、上述の膜沸騰ガスを発生させて、上記(i)と(ii)の一方又は両方により、セラミックス基複合材料のマトリックスの気孔においてセラミックスを堆積させてもよい。この場合、例えば、図2Aと図3において、加熱体1が省略され、セラミックス基複合材料10の数が1つになり、1つのセラミックス基複合材料10が上方と下方から多孔体3に接触し、断熱材5は、セラミックス基複合材料10の外周10aを覆い、他の点は、上述と同じであってよい。また、加熱体1の省略に加えて、又は加熱体1の省略の代わりに、断熱板2を省略してもよい。
Claims (9)
- マトリックスと、前記マトリックス内に設けられた強化繊維とを備えるセラミックス基複合材料の製造方法であって、
(A)強化繊維により構成された繊維体に、前記マトリックスの一部となるセラミックス材料の粉末を含浸させ、
(B)前記粉末が含浸させられた前記繊維体を前記マトリックスの液体原料内に配置し、
(C)この状態で前記繊維体を加熱することにより、前記液体原料を膜沸騰状態にして、前記液体原料に由来するセラミックスを前記マトリックスの一部として前記繊維体内に生じさせる、セラミックス基複合材料の製造方法。 - 前記(C)では、
(C1)前記繊維体を加熱することにより、前記液体原料を前記膜沸騰状態にして、前記セラミックスを前記繊維体内に生じさせ、
(C2)前記繊維体を前記液体原料の沸点より低い温度まで冷却し、
前記(C1)と前記(C2)を繰り返す、請求項1に記載のセラミックス基複合材料の製造方法。 - 前記(A)では、
(A1)前記粉末を液体と混合することによりスラリーを生成し、
(A2)スラリー容器内で前記スラリー内に前記繊維体が埋まった状態にし、
(A3)前記スラリー容器の内部を真空引きして、前記粉末を含有する前記スラリーを前記繊維体の内部に含浸させる、請求項1又は2に記載のセラミックス基複合材料の製造方法。 - 前記(A)で用いる前記粉末のメディアン径は、1μm以上20μm以下である、請求項1~3のいずれか一項に記載のセラミックス基複合材料の製造方法。
- 前記(A)で用いる前記粉末は、メディアン径が5μmの粉末と、メディアン径が17μmの粉末との混合粉末である、請求項1~4のいずれか一項に記載のセラミックス基複合材料の製造方法。
- 前記(C)では、前記液体原料を保持する処理容器の内部において、前記繊維体と加熱体を配置し、
前記(C)では、前記加熱体を誘導加熱することにより、前記繊維体を加熱する、請求項1~5のいずれか一項に記載のセラミックス基複合材料の製造方法。 - 前記(C)では、前記処理容器の外部に配置したコイルに交流電流を流すことで当該コイルが発生する交流磁場により、前記加熱体を誘導加熱し、誘導加熱された前記加熱体により前記繊維体を加熱し、
前記処理容器は、非導電性材料により形成されている、請求項6に記載のセラミックス基複合材料の製造方法。 - 前記(C)では、取付具により、前記繊維体は前記加熱体に取り付けられており、前記取付具と前記繊維体と前記加熱体が、前記処理容器の内面に接触しないように吊り下げられている、請求項6又は7に記載のセラミックス基複合材料の製造方法。
- 請求項1~8のいずれか一項に記載のセラミックス基複合材料の製造方法により製造されたセラミックス基複合材料。
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