WO2019176896A1 - Procédé de production d'un matériau composite de céramique imprégné de silicium, procédé de production d'une plaque de frottement et procédé de production de disque de frein - Google Patents

Procédé de production d'un matériau composite de céramique imprégné de silicium, procédé de production d'une plaque de frottement et procédé de production de disque de frein Download PDF

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WO2019176896A1
WO2019176896A1 PCT/JP2019/009860 JP2019009860W WO2019176896A1 WO 2019176896 A1 WO2019176896 A1 WO 2019176896A1 JP 2019009860 W JP2019009860 W JP 2019009860W WO 2019176896 A1 WO2019176896 A1 WO 2019176896A1
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temperature
silicon
ceramic
ceramic composite
producing
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PCT/JP2019/009860
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Japanese (ja)
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野呂　匡志
高木　俊
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イビデン株式会社
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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
    • C04B35/71—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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D65/00—Parts or details
    • F16D65/02—Braking members; Mounting thereof
    • F16D65/12—Discs; Drums for disc brakes

Definitions

  • the present invention relates to a method for producing a silicon-impregnated ceramic composite, a method for producing a friction plate, and a method for producing a brake disk.
  • an impermeable heat-resistant structural composite material disclosed in Patent Document 1 is known.
  • the impermeable heat-resistant structural composite material of Patent Document 1 is composed of a porous base material including a matrix made of carbon and silicon carbide and refractory fibers, and silicon impregnated in the porous base material.
  • Such a silicon-impregnated ceramic composite has mechanical properties suitable for constituting a structural element, and can retain the mechanical properties even at high temperatures.
  • the silicon-impregnated ceramic composite material disclosed in Patent Document 1 is manufactured as follows. First, a porous substrate (ceramic composite material) is obtained by forming a matrix for a fiber reinforcement formed by combining refractory fibers. The matrix is heated by impregnating the fiber reinforcement with a liquid composition containing a precursor to a gas process that deposits pyrolytic carbon and silicon carbide on the fiber of the fiber reinforcement by chemical vapor infiltration. Formed by a liquid process that converts precursors to carbon or silicon carbide. Next, the porous base material is impregnated with molten metal silicon using a capillary phenomenon.
  • Patent Document 1 In the manufacturing method disclosed in Patent Document 1, it is necessary to form a ceramic composite material in advance before impregnation with metallic silicon. For this reason, two heat treatments are required when forming the ceramic composite (forming a matrix) and impregnating the metal silicon, and the manufacturing work is complicated.
  • the present invention has been made in view of such circumstances, and an object thereof is to simplify the manufacturing process of a silicon-impregnated ceramic composite material such as a friction plate and a brake disk.
  • a method for producing a silicon-impregnated ceramic composite material for achieving the above object comprises heating a molded body containing ceramic fibers and a ceramic precursor, and ceramicizing the ceramic precursor to obtain a ceramic composite material.
  • a method for producing a silicon-impregnated ceramic composite material comprising: a step of impregnating the ceramic composite material with metal silicon, wherein the molded body is inserted into a container containing solid metal silicon via a support. The temperature in the container is set to a second temperature equal to or higher than the melting point of the metal silicon after the firing step is performed with the temperature at which the ceramic precursor is ceramicized and a first temperature lower than the melting point of the metal silicon.
  • the ceramic composite material is impregnated with molten metal silicon through the support made of a porous material by raising the temperature. Carry out the serial impregnation step.
  • the ceramic precursor contained in the molded body is converted to ceramic and a ceramic composite having voids is obtained. Since the 1st temperature at this time is a temperature below melting
  • the first temperature is preferably a temperature of 500 ° C. or higher and 1400 ° C. or lower
  • the second temperature is preferably a temperature of 1410 ° C. or higher and 2000 or lower.
  • the ceramic precursor can be ceramic while suppressing the metal silicon from melting and impregnating into the molded body more preferably during the heat treatment at the first temperature corresponding to the firing step. At the same time, voids can be formed.
  • the metal silicon can be preferably impregnated into the voids of the ceramic composite material at the time of the heat treatment at the second temperature corresponding to the impregnation step, and excessive heating is performed. It is possible to suppress deterioration due to being performed.
  • the ceramic fiber is preferably at least one selected from carbon fibers and silicon carbide fibers. According to the said structure, based on the property of carbon and silicon carbide with high affinity with respect to metallic silicon, it becomes easy to impregnate a metallic composite with a metallic silicon in an impregnation process. As a result, a dense silicon-impregnated ceramic composite with few voids can be obtained.
  • the ceramic precursor is at least one selected from a carbon-based precursor that becomes carbon by heating and a silicon carbide-based precursor that becomes silicon carbide by heating. preferable.
  • a ceramic composite material having a matrix (porous matrix) made of at least one of carbon and silicon carbide while forming voids in the firing step can be obtained. Therefore, based on the properties of carbon and silicon carbide having high affinity for metallic silicon, metallic silicon is easily impregnated in the voids of the ceramic composite material in the impregnation step. As a result, a dense silicon-impregnated ceramic composite with few voids can be obtained.
  • the temperature in the container is changed from the first temperature to the second temperature based on a change in decomposition gas derived from the ceramic precursor contained in the molded body. It is preferable to raise the temperature.
  • the heating time at the first temperature is insufficient or excessive. That is, when the molded body is heated at the first temperature, the ceramic precursor contained in the molded body is converted into ceramic. Along with this ceramization, decomposition gas derived from the ceramic precursor is generated. Therefore, by raising the temperature from the first temperature to the second temperature based on the generation state of the decomposition gas derived from the ceramic precursor, the heating time at the first temperature can be set to any state in which the progress of ceramization of the ceramic precursor is arbitrary ( For example, it can be easily adjusted to the time when it becomes a completely ceramicized state.
  • a friction plate manufacturing method for achieving the above object includes the above silicon impregnated ceramic composite manufacturing method. According to the said structure, the manufacturing process of a friction board can be simplified.
  • a brake disk manufacturing method for achieving the above object includes the above silicon impregnated ceramic composite manufacturing method. According to the said structure, the manufacturing process of a brake disc can be simplified.
  • the manufacturing process of the silicon-impregnated ceramic composite can be simplified.
  • (A) is a schematic diagram of a fiber structure
  • (b) is a schematic diagram of a molded body
  • (c) is a schematic diagram of a ceramic composite material
  • (d) is a schematic diagram of a silicon-impregnated ceramic composite material.
  • Explanatory drawing which shows the state which has arrange
  • the graph which shows the temperature change in a container.
  • the silicon-impregnated ceramic composite material is manufactured by sequentially performing a molding process, a firing process, and an impregnation process described below.
  • the forming step is a step of forming a formed body containing ceramic fibers and a ceramic precursor.
  • a fiber structure 12 constituting an aggregate part of a formed body is formed by combining a plurality of ceramic fibers 11.
  • the formation method of the fiber structure 12 is not specifically limited, The well-known method used when manufacturing a silicon impregnation ceramic composite material can be used. Examples of the known method include a method in which sheet-like two-dimensional fiber layers such as a woven fabric and a nonwoven fabric are stacked, and a method using three-dimensional weaving.
  • FIG. 1A a fiber structure 12 formed by stacking a plurality of ceramic fibers 11 is illustrated.
  • the ceramic fiber 11 examples include carbon fiber, silicon carbide fiber, alumina fiber, and mullite fiber. Among these, carbon fiber and silicon carbide fiber are particularly preferable from the viewpoint of improving the impregnation efficiency of metal silicon in the impregnation step described later.
  • the fiber structure 12 may be composed of a kind of ceramic fibers 11 or may be composed of a plurality of kinds of ceramic fibers 11.
  • the diameter of the ceramic fiber 11 is, for example, 5 to 30 ⁇ m.
  • the gap between the fibers of the fiber structure 12 and the surface of the fiber structure 12 are filled with a filler containing a ceramic precursor as a main component.
  • Form body 13a The molded body 13a includes a skeleton portion 14 constituted by the fiber structure 12 and a matrix portion 15a constituted by a ceramic precursor (filler).
  • the ceramic precursor is a precursor used in a polymer impregnation firing method (PIP method).
  • the ceramic precursor include a carbon-based precursor that becomes carbon by heating, a silicon carbide-based precursor that becomes silicon carbide by heating, and a metal alkoxide precursor that becomes an oxide-based ceramic by heating.
  • the carbon precursor include pitch, phenol resin, furan resin, polyvinyl alcohol, and copna resin.
  • the silicon carbide precursor include polycarbosilane and derivatives thereof, and a mixture of a siloxane resin and a carbon precursor.
  • the metal alkoxide precursor include sodium methoxide, sodium ethoxide, potassium t-butoxide and the like.
  • a carbon-based precursor, a silicon carbide-based precursor, and a combined use of a carbon-based precursor and a silicon carbide-based precursor are particularly preferable.
  • the filler may be composed of a kind of ceramic precursor or may be composed of a plurality of kinds of ceramic precursors.
  • the ceramic precursor contained in the molded body 13a is thermosetting, it is preferably cured in advance before the firing step. By pre-curing, deformation due to softening can be prevented in the firing step.
  • the curing method is not particularly limited, and a method using a reaction catalyst, a thermal curing method, and the like can be used.
  • thermosetting refers to a resin in which a monomer is bonded in a network and does not flow even when heated, and is said to be thermosetting even if it can be cured by a method other than heating.
  • the filler may contain other components other than the ceramic precursor such as a solvent and ceramic powder.
  • the firing step is a step of obtaining the ceramic composite material 13b by converting the ceramic precursor contained in the molded body 13a into a ceramic by heating.
  • the ceramic composite material 13b has the frame
  • the matrix portion 15b has voids formed as the ceramic precursor is converted into ceramics, and the ceramic composite material 13b is a porous body having the voids.
  • the impregnation step is a step of obtaining the silicon-impregnated ceramic composite material 13c by impregnating the voids of the ceramic composite material 13b with metal silicon melted by heating.
  • the silicon-impregnated ceramic composite material 13c has a skeleton portion 14 composed of a fiber structure 12, and a matrix portion 15c composed of ceramic derived from a ceramic precursor and metallic silicon. It is a dense body.
  • a baking process and an impregnation process are continuously performed by the multistep heat processing by a different temperature range.
  • the molded body 13a is placed in a bottomed box-like heat-resistant container 20 made of ceramic or the like.
  • the molded body 13 a is placed in the container 20 via the support tool 21 by being placed on the support tool 21 placed on the bottom surface of the container 20.
  • the support tool 21 is formed in such a size and shape as to contact only a part of the lower surface of the molded body 13a, and supports the molded body 13a at one or several points on the lower surface of the molded body 13a.
  • the support tool 21 may be singular or plural.
  • Examples of the shape of the support 21 include a prismatic shape, a cylindrical shape, a truncated pyramid shape, and a truncated cone shape.
  • a truncated pyramid shape and a truncated cone shape are particularly preferable because the number of contacts with the lower surface of the molded body 13a can be reduced.
  • the support 21 is made of a porous material having continuous pores with a size that causes a capillary phenomenon.
  • the porous material constituting the support 21 include a porous material made of silicon carbide and a porous material made of carbon such as graphite.
  • the porosity of the porous material constituting the support 21 is, for example, 20 to 60%.
  • a solid metal silicon 22 such as powder, granule or lump is disposed in the gap S between the bottom surface of the container 20 and the molded body 13a placed on the support 21.
  • the purity of metallic silicon is, for example, 95% or more.
  • the amount of the metal silicon 22 accommodated in the container 20 is, for example, an amount corresponding to the sum of the pore volume of the ceramic composite 13b and the pore volume of the support 21 (for example, 1.00 to 1.05 times the sum)
  • the amount corresponding to the volume of in this case, the porosity of the silicon-impregnated ceramic composite material 13c can be close to 0%.
  • the usage-amount of the metal silicon 22 can be suppressed and manufacturing cost can be suppressed.
  • the container 20 is used in an inert atmosphere such as argon or nitrogen or in vacuum using a known heating means such as a firing furnace. Heat. At this time, the container 20 is heated in multiple stages at different temperature ranges.
  • the temperature in the container 20 is raised to the first temperature, and the primary heating is performed by holding the temperature at the first temperature for a certain period of time. Thereafter, the temperature in the container 20 is raised to a second temperature higher than the first temperature, and is maintained for a certain period of time to perform secondary heating. Thereafter, the temperature in the container 20 is lowered.
  • Primary heating is a heat treatment corresponding to the firing step.
  • the first temperature of the primary heating is a temperature at which the ceramic precursor is ceramicized and a temperature lower than the melting point of metal silicon, and is set according to the type of the ceramic precursor contained in the molded body 13a.
  • the ceramic precursor contained in the molded body 13a is thermally decomposed and converted into ceramic, and voids are formed.
  • the molded body 13a becomes the ceramic composite material 13b.
  • the temperature (first temperature) in the container 20 is a temperature lower than the melting point of the metal silicon, the metal silicon 22 accommodated in the container 20 is maintained in a solid state.
  • the first temperature is, for example, preferably 500 ° C. or more and 1400 ° C. or less, more preferably 1200 ° C. or more and 1350 ° C. or less.
  • the ceramic precursor can be converted into a ceramic and voids can be formed at the same time while suppressing melting of the metal silicon 22.
  • the primary heating is preferably performed until the ceramic precursor contained in the molded body 13a is sufficiently ceramicized. Whether or not the ceramic precursor is sufficiently ceramicized can be determined based on, for example, a change in decomposition gas generated from the molded body 13a. That is, when the ceramic precursor is ceramized by heating, a decomposition gas accompanying the thermal decomposition of the ceramic precursor is generated. Therefore, by measuring this cracked gas, the total amount of cracked gas generated, the amount of change in cracked gas generated per unit time, the concentration and type of cracked gas in the furnace, the concentration of cracked gas per unit time Based on the amount of change or the like, it can be determined that the ceramic precursor contained in the molded body 13a has been sufficiently ceramicized (for example, 90% or more).
  • Secondary heating is a heat treatment corresponding to the impregnation step.
  • the second temperature of the secondary heating is set to be equal to or higher than the melting point of metal silicon.
  • the silicon silicon 22 accommodated in the container 20 is melted by the secondary heating.
  • the melted metal silicon enters the void of the ceramic composite material 13b through the support 21 made of a porous material by capillary action, and the void is impregnated with the metal silicon 22.
  • the ceramic composite material 13b becomes a silicon-impregnated ceramic composite material 13c impregnated with the metal silicon 22.
  • the second temperature is preferably a temperature of 1410 ° C. or higher and 2000 ° C. or lower, for example. By setting the temperature range, it is possible to more reliably impregnate metal silicon while suppressing deterioration of the skeleton portion 14 and the matrix portion 15b of the ceramic composite material 13b due to exposure to a high temperature.
  • the secondary heating is preferably performed until the metal silicon is sufficiently impregnated into the voids present in the ceramic composite material 13b.
  • the amount of the metal silicon 22 accommodated in the container 20 is an amount corresponding to the sum of the pore volume of the ceramic composite material 13b and the pore volume of the support 21, all the metal silicon 22 is impregnated. Therefore, it can be determined that the metal silicon is sufficiently impregnated.
  • the temperature in the container 20 is lowered, the silicon-impregnated ceramic composite material 13c is taken out from the container 20, and the support 21 integrated on the lower surface of the silicon-impregnated ceramic composite material 13c is separated. Thereby, the silicon-impregnated ceramic composite material 13c is obtained.
  • the use of the silicon-impregnated ceramic composite material 13c manufactured by the manufacturing method of the present embodiment is not particularly limited, but can be applied as a friction plate such as a brake disk or a clutch disk. Therefore, the manufacturing method of this embodiment can also be applied as one process when manufacturing friction plates, such as a brake disk and a clutch disk.
  • a method for producing a silicon-impregnated ceramic composite includes a firing step in which a ceramic composite is obtained by heating a molded body containing ceramic fibers and a ceramic precursor to ceramicize the ceramic precursor; An impregnation step of impregnating the material with metallic silicon.
  • a molded body is placed through a support in the interior of a container containing solid metallic silicon. The container was melted by raising the temperature in the container to a second temperature equal to or higher than the melting point of the metal silicon after performing the firing step with the temperature at which the ceramic precursor is ceramicized and a first temperature lower than the melting point of the metal silicon.
  • An impregnation step of impregnating the ceramic composite material with metal silicon through a support made of a porous material is performed.
  • the firing process and the impregnation process can be continuously performed in one heat treatment by the temperature control in the container, and as a result, the manufacturing process of the silicon-impregnated ceramic composite is simplified. .
  • the first temperature is a temperature of 500 ° C. or higher and 1400 ° C. or lower.
  • the ceramic precursor in the primary heating corresponding to the firing step, more preferably, is made into a ceramic and simultaneously formed voids while suppressing the metal silicon from melting and impregnating the molded body. it can.
  • the second temperature is a temperature of 1410 ° C. or higher and 2000 ° C. or lower. According to the said structure, in the secondary heating corresponded to an impregnation process, while the metal silicon impregnation to the space
  • the ceramic fiber is at least one selected from carbon fiber and silicon carbide fiber. According to the said structure, based on the property of carbon and silicon carbide with high affinity with respect to a metal silicon, it becomes easy to impregnate a ceramic composite material with a metal silicon in an impregnation process. As a result, a dense silicon-impregnated ceramic composite with few voids can be obtained.
  • the ceramic precursor is at least one selected from a carbon-based precursor that becomes carbon by heating and a silicon carbide-based precursor that becomes silicon carbide by heating.
  • the ceramic composite material which has a matrix (porous matrix) which consists of at least one of carbon and silicon carbide, forming a space
  • the temperature in the container is raised from the first temperature to the second temperature based on the change in the decomposition gas derived from the ceramic precursor contained in the compact.
  • the heating time by the first temperature is increased by the progress of ceramization of the ceramic precursor. It can be easily adjusted to the time when it becomes an arbitrary state (for example, a completely ceramicized state). Therefore, it can suppress that the heating time by 1st temperature runs short or becomes excessive.
  • the heating time at the first temperature can be easily adjusted to the time when the ceramic precursor is sufficiently ceramicized. Therefore, the impregnation step is performed by raising the temperature to the second temperature in a state where the ceramic precursor is not sufficiently ceramicized, and heating at the first temperature is continued even after the ceramic precursor is sufficiently ceramicized. This can be suppressed.
  • the molded body 13a is formed by filling the fiber structure 12 formed by combining the ceramic fibers 11 with the filler containing the ceramic precursor. Is not limited to this. For example, after the fiber structure 12 is filled with a filler, a processing such as cutting may be performed to obtain the formed body 13a. Moreover, you may form the molded object 13a by shape
  • the support tool 21 comprised by the porous material
  • the support tool 21 performs the secondary heating (impregnation process)
  • the support tool 21 is also made into a ceramic as well as the molded body 13a and a void is formed to form the support tool 21 having a porous structure.
  • the support 21 may be formed integrally with the molded body 13a, and the molded body 13a having the support 21 may be placed directly on the container 20.
  • the method of setting the timing which raises the temperature in the container 20 from 1st temperature to 2nd temperature For example, the heating time during which the progress of ceramization of the ceramic precursor contained in the molded body 13a is in an arbitrary state is measured by a preliminary test in advance, and the temperature in the container 20 is set as the heating time elapses. The temperature may be raised from the first temperature to the second temperature.
  • the primary heating corresponding to a baking process may change the temperature in the range of 1st temperature.
  • the temperature in the container 20 may be continuously increased to the second temperature, and the period of staying in the first temperature range (first temperature range) in the middle may be primary heating.
  • the temperature rise curve in the container 20 it is preferable to adjust the temperature rise curve in the container 20 so that a sufficient period of staying in the first temperature range is ensured.
  • the temperature may be changed in the second temperature range.
  • a disk-shaped formed body having a diameter of 300 mm and a thickness of 10 mm is formed by filling the gap and the surface of the fiber structure in which ceramic fibers are stacked with each other.
  • the ceramic fiber a plain woven fabric using silicon carbide fibers having a diameter of 12 ⁇ m is used, and five woven fabrics are laminated and used as an aggregate.
  • the obtained aggregate is impregnated with a liquid phenol resin as a filler, and then put in a dryer to be cured. In the dryer, the phenolic resin can be thermally cured, and a molded body that is not thermally deformed in the subsequent baking step can be obtained.
  • the compact is disposed through a support made of a porous material of silicon carbide, and powdered metallic silicon is disposed. Then, using a firing furnace, the container containing the compact and the metal silicon is subjected to a two-stage heat treatment at a first temperature and a second temperature as shown in FIG. 3 in an argon atmosphere.
  • a silicon-impregnated ceramic composite material can be obtained.
  • the temperature conditions for the heat treatment are as follows.
  • First temperature 1300 ° C Heating time by first temperature: 60 minutes Second temperature: 1500 ° C Heating time at second temperature: 20 minutes
  • the decomposition gas continues to be generated from the phenol resin (ceramic precursor) until the temperature rises to the first temperature and while the temperature is maintained at the first temperature, but the generation of the decomposition gas converges with time. After confirming that the generation of cracked gas has converged, the temperature is raised to the second temperature. At the second temperature, the metallic silicon filled in the ceramic container is melted, and the ceramic composite material is impregnated by transferring the support made of a porous material, and firing and silicon impregnation can be performed continuously. .
  • the ceramic precursor is thermally cured in the firing step, and deformation during firing can be prevented.

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Abstract

L'invention concerne un procédé de production d'un matériau composite de céramique imprégné de silicium qui comprend : une étape de cuisson dans laquelle un article moulé comprenant des fibres de céramique et un précurseur de céramique est chauffé, et un matériau composite céramique est obtenu par conversion du précurseur de céramique en une céramique ; et une étape d'imprégnation dans laquelle un silicium métallique est imprégné dans le matériau composite de céramique. L'article moulé est placé à l'intérieur d'un récipient qui contient le silicium métallique solide avec un outil de support entre eux. Après que l'étape de cuisson ait été effectuée à une première température, qui est la température à l'intérieur du récipient et qui est une température inférieure au point de fusion du silicium métallique et à laquelle le précurseur de céramique est converti en une céramique, l'étape d'imprégnation est effectuée, dans laquelle, en élevant la température à une seconde température, qui est une température supérieure ou égale au point de fusion du silicium métallique, le silicium métallique fondu s'imprègne dans le matériau composite céramique par l'intermédiaire de l'outil de support, qui comprend un matériau poreux.
PCT/JP2019/009860 2018-03-13 2019-03-12 Procédé de production d'un matériau composite de céramique imprégné de silicium, procédé de production d'une plaque de frottement et procédé de production de disque de frein WO2019176896A1 (fr)

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JP2018-045691 2018-03-13
JP2018045691A JP7049869B2 (ja) 2018-03-13 2018-03-13 シリコン含浸セラミック複合材の製造方法、摩擦板の製造方法、及びブレーキディスクの製造方法

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CN113526971A (zh) * 2021-06-10 2021-10-22 浙江理工大学 一种海绵状碳化硅纳米纤维预制体制备SiC陶瓷基复合材料的方法
CN113526971B (zh) * 2021-06-10 2022-12-02 浙江理工大学 一种海绵状碳化硅纳米纤维预制体制备SiC陶瓷基复合材料的方法
CN116375487A (zh) * 2023-04-03 2023-07-04 合肥富维康新材料有限公司 一种低孔隙率SiC纤维单向预浸带的制备方法

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