WO2022210470A1 - 接合体の製造方法 - Google Patents

接合体の製造方法 Download PDF

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Publication number
WO2022210470A1
WO2022210470A1 PCT/JP2022/014812 JP2022014812W WO2022210470A1 WO 2022210470 A1 WO2022210470 A1 WO 2022210470A1 JP 2022014812 W JP2022014812 W JP 2022014812W WO 2022210470 A1 WO2022210470 A1 WO 2022210470A1
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WIPO (PCT)
Prior art keywords
interior
contact surface
silicon
outer layer
silicon carbide
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Ceased
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PCT/JP2022/014812
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English (en)
French (fr)
Inventor
雅彦 堀内
威男 馬目
信也 宮崎
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Kyocera Corp
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Kyocera Corp
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Priority to US18/553,323 priority Critical patent/US20240182369A1/en
Priority to JP2023511223A priority patent/JPWO2022210470A1/ja
Priority to EP22780681.7A priority patent/EP4317111A4/en
Publication of WO2022210470A1 publication Critical patent/WO2022210470A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Definitions

  • the present invention relates to a method for manufacturing a joined body.
  • Patent Document 1 discloses a method of forming an oxide film in advance only on the non-joining surfaces of the silicon carbide ceramic materials when joining the silicon carbide ceramic materials together using a brazing filler metal containing silicon. Have been described. By such a method, the pores or grooves are not clogged even when the silicon carbide ceramic materials are joined together on the surfaces having the pores or grooves.
  • a method for manufacturing a joined body includes a first outer layer portion located on the outer surface side and containing silicon oxide as a main component, and a first inner portion containing silicon carbide and silicon surrounded by the first outer layer portion. a step of obtaining a composite; obtaining a second composite having a second outer layer portion located on the outer surface side and containing silicon oxide as a main component, and a second inner portion containing silicon carbide and silicon surrounded by the second outer layer portion.
  • FIG. 3 is an explanatory diagram showing a joined body obtained by a manufacturing method according to an embodiment of the present disclosure
  • FIG. 4 is an explanatory diagram showing steps of a manufacturing method according to an embodiment of the present disclosure
  • the conventional joining method uses a brazing material, so there is a brazing material layer between the silicon carbide ceramic materials.
  • a brazing material layer between the silicon carbide ceramic materials.
  • the presence of voids in the brazing material layer reduces the joint strength.
  • silicon carbide ceramic materials are joined together by vacuum brazing. Therefore, the carbon contained in the brazing filler metal may scatter and stain the furnace wall.
  • a bonded body having excellent bonding strength and a method for manufacturing a bonded body having excellent bonding strength without staining the furnace wall are desired.
  • the method for manufacturing a joined body according to the present disclosure includes the step of contacting the first contact surface and the second contact surface and performing heat treatment in a vacuum atmosphere or an inert gas atmosphere. Therefore, according to the present disclosure, it is possible to provide a method for manufacturing a bonded body having excellent bonding strength without contaminating the walls of the furnace.
  • a joined body obtained by a manufacturing method according to an embodiment of the present disclosure includes the first composite and the second composite as described above. Prepare. A bonded body according to the present disclosure will be described based on FIG.
  • a joined body 10 includes a first composite 1 and a second composite 2.
  • the first composite 1 has a first outer layer 11 and a first interior 12 surrounded by the first outer layer 11 .
  • the first outer layer portion 11 is located on the outer surface side of the first composite 1 and contains silicon oxide as a main component.
  • the first outer layer portion 11 is an oxide film containing silicon oxide as a main component, and its thickness is not limited.
  • the first outer layer portion 11 has a thickness of, for example, 700 nm or more and 900 nm or less.
  • Main component as used herein means a component that accounts for 80% by mass or more.
  • the components are identified by an X-ray diffractometer using CuK ⁇ rays, and the content of silicon carbide and silicon can be obtained by, for example, the Rietveld method.
  • the first interior 12 contains silicon carbide and silicon and is surrounded by the first outer layer portion 11 .
  • an oxide film mainly composed of silicon oxide formed by oxidizing the outer surface of the member corresponds to the "first outer layer portion 11"
  • the remaining portion corresponds to the "first interior 12”.
  • the contents of silicon carbide and silicon contained in the first interior 12 are not limited.
  • Silicon carbide may be contained, for example, at a rate of 70% by mass or more and 92% by mass or less. Silicon carbide is superior to silicon in mechanical properties such as Young's modulus (dynamic modulus) and three-point bending strength. Therefore, when the content of silicon carbide is 70% by mass or more, the mechanical properties of the resulting joined body are improved.
  • silicon has higher thermal conductivity than silicon carbide. Therefore, when the content of silicon carbide is 92% by mass or less, the thermal conductivity of the resulting joined body is improved. Therefore, if the content of silicon carbide is 70% by mass or more and 92% by mass or less, both mechanical properties and thermal conductivity can be achieved.
  • the difference between the average distance between the centers of gravity of silicon and the average circle-equivalent diameter of silicon is not limited, and may be, for example, 8 ⁇ m or more and 20 ⁇ m or less.
  • this difference is 8 ⁇ m or more, the distribution density of silicon carbide increases. Therefore, the rigidity of the resulting joined body is improved, and the unevenness of rigidity is reduced.
  • this difference is 20 ⁇ m or less, the resulting joined body has improved thermal conductivity, and uneven thermal conductivity is reduced.
  • the closed porosity of the first interior 12 is not limited, and may be, for example, 0.1% or less. If the closed porosity of the first interior 12 is 0.1% or less, the closed pore volume is reduced. Therefore, even if particles are contained in the closed pores in the resulting joined body, the risk of silicon being eroded by the particles is reduced.
  • the second composite 2 has a second outer layer portion 21 and a second inner portion 22 surrounded by the second outer layer portion 21 .
  • the second outer layer portion 21 is located on the outer surface side of the second composite 2 and contains silicon oxide as a main component.
  • the second outer layer portion 21 is an oxide film containing silicon oxide as a main component, and its thickness is not limited.
  • the second outer layer portion 21 has a thickness of, for example, 700 nm or more and 900 nm or less.
  • the “main component” is as described above, and detailed description is omitted.
  • the second interior 22 contains silicon carbide and silicon and is surrounded by the second outer layer portion 21 .
  • an oxide film mainly composed of silicon oxide formed by oxidizing the outer surface of the member corresponds to the "second outer layer portion 21"
  • the remaining portion corresponds to the "second interior 22".
  • the contents of silicon carbide and silicon contained in the second interior 22 are not limited. Silicon carbide may be contained, for example, at a rate of 70% by mass or more and 92% by mass or less. Silicon carbide is superior to silicon in mechanical properties such as Young's modulus (dynamic modulus) and three-point bending strength. Therefore, when the content of silicon carbide is 70% by mass or more, the mechanical properties of the resulting joined body are improved. On the other hand, silicon has higher thermal conductivity than silicon carbide. Therefore, when the content of silicon carbide is 92% by mass or less, the thermal conductivity of the resulting joined body is improved. Therefore, if the content of silicon carbide is 70% by mass or more and 92% by mass or less, both mechanical properties and thermal conductivity can be achieved.
  • Each component contained in the first interior 21 and the second interior 22 may be identified by an X-ray diffractometer, and each content of silicon carbide and silicon may be obtained by the Rietveld method.
  • the difference between the average distance between the centroids of silicon and the average circle-equivalent diameter of silicon is not limited, and may be, for example, 8 ⁇ m or more and 20 ⁇ m or less.
  • this difference is 8 ⁇ m or more, the distribution density of silicon carbide increases. Therefore, the rigidity of the resulting joined body is improved, and the unevenness of rigidity is reduced.
  • this difference is 20 ⁇ m or less, the resulting joined body has improved thermal conductivity, and uneven thermal conductivity is reduced.
  • the distance between the centers of gravity of silicon in the first interior 21 and the second interior 22 may be obtained by the following method. First, a part of each of the first interior 21 and the second interior 22 is cut out. After cutting out, diamond abrasive grains are used to select an average range from the mirror surface obtained by polishing the cross section. After that, a range having an area of 0.191 mm 2 (horizontal length of 351 ⁇ m, vertical length of 545 ⁇ m) is photographed with a scanning electron microscope to obtain an observed image.
  • the image analysis software "Azo-kun (ver 2.52)" registered trademark, manufactured by Asahi Kasei Engineering Co., Ltd.
  • the distance between the centers of gravity of silicon is obtained by a method called the distance between the centers of gravity of dispersion measurement using an image analysis software manufactured by Co., Ltd.
  • the setting conditions for this method are a threshold of 190 to 195, which is an index indicating the brightness of the image, a light brightness, a small figure removal area of 1 ⁇ m 2 , and a noise removal filter.
  • the circle-equivalent diameter of silicon is obtained by a technique called particle analysis, using the observation image as a target.
  • the setting conditions for this method are the same as those used in the centroid distance method.
  • the closed porosity of the second interior 22 is not limited, and may be, for example, 0.1% or less. If the closed porosity of the second interior 22 is 0.1% or less, the closed pore volume is reduced. Therefore, even if particles are contained in the closed pores in the resulting joined body, the risk of silicon being eroded by the particles is reduced.
  • the circle-equivalent diameter of silicon can be obtained by a technique called particle analysis, using the observation image as a target.
  • the setting conditions for this method are a threshold of 155, which is an index indicating the brightness of an image, a brightness of dark, a small figure removal area of 1 ⁇ m 2 , and a noise removal filter.
  • first composite body 1 and the second composite body 2 have the first outer layer portion 11 and the second outer layer portion 21, respectively, even if the joined body 10 is exposed to high temperature conditions, the first inner portion 12 and the second 2.
  • the shape stability of the interior 22 is improved. The reason is that the melting point of silicon oxide is higher than that of silicon.
  • the first contact surface 15 on which the first interior 12 contacts the second interior 22 and the second contact surface 25 on which the second interior 22 contacts the first interior 12 are: , are diffusion bonded. Diffusion bonding is to join members together without using an adhesive or the like. The members are brought into close contact with each other, and under temperature conditions below the melting point of the members, diffusion of atoms occurring between the joint surfaces is used. It is to join the members together.
  • silicon atoms (Si) are diffused and joined to the first contact surface 15 and the second contact surface 25 .
  • the joined body 10 In the joined body 10 according to one embodiment, no gap is included between the first contact surface 15 and the second contact surface 25 . Since the first contact surface 15 and the second contact surface 25 are diffusion-bonded and no gap is included between the first contact surface 15 and the second contact surface 25, the joined body 10 is excellent. It has excellent bonding strength. Furthermore, in the joined body 10, heat exchange between the first interior 12 and the second interior 22 is easily performed.
  • the maximum length in the thickness direction between the first contact surface 15 and the second contact surface 25 is It means that it does not contain voids larger than 20 ⁇ m. Therefore, even when only fine voids with a maximum length of 20 ⁇ m or less are included, this corresponds to “not including voids”.
  • voids for example, a mirror surface obtained by polishing a cross section including the first contact surface 15 and the second contact surface 25 may be observed with a scanning electron microscope at a magnification of about 250 times. The length of the first contact surface (second contact surface) on the mirror surface is assumed to be 0.35 mm, for example, and the maximum length of the gap at this length is measured.
  • the first contact surface 15 may be provided with a first concave portion 13 extending in the depth direction, as shown in FIG.
  • a first concave portion 13 By providing such a first concave portion 13 , the fluid can flow through the first concave portion 13 of the joined body 10 to be obtained.
  • the width and depth of the first recess 13 can be appropriately adjusted according to the speed and viscosity of the fluid. Therefore, the effect of the fillet in the first recess 13 (for example, the generation of fluid turbulence caused by the fillet) is reduced to a negligible level. As a result, even if the fluid is caused to flow through the first concave portion 13, variations in flow path resistance can be reduced.
  • the size and shape of the first concave portion 13 are not limited, and may be appropriately set according to the size of the joined body 10, application, type of fluid to be flowed, and the like. Furthermore, a through hole (first through hole) may be used instead of the first recess 13 .
  • At least one of the inner wall surface and the inner bottom surface of the first recess 13 or the inner wall surface of the first through hole may be provided with a first inner layer portion 14 containing silicon oxide as a main component.
  • a first inner layer portion 14 containing silicon oxide as a main component.
  • the second contact surface 25 may be provided with a second concave portion 23 extending in the depth direction, as shown in FIG.
  • the fluid can flow through the second recesses 23 of the resulting joined body 10 .
  • the second recess 23 as in the first recess 13 , even if the fluid is allowed to flow through the second recess 23 , variations in the flow path resistance can be reduced.
  • the size and shape of the second concave portion 23 are not limited, and may be appropriately set according to the size of the joined body 10, application, type of fluid to be flowed, and the like. Furthermore, a through hole (second through hole) may be used instead of the second recess 23 .
  • At least one of the inner wall surface and the inner bottom surface of the second recess 23 or the inner wall surface of the second through hole may be provided with a second inner layer portion 24 containing silicon oxide as a main component.
  • the reason is as explained in the first recess 13 above.
  • the second inner layer portion 24 may have a thickness of, for example, 700 nm or more and 900 nm or less.
  • the first recess 13 (or first through hole) and the second recess 23 (or first through hole) may have the same shape or different shapes. Furthermore, the first recess 13 (or the first through hole) and the second recess 23 (or the first through hole) join the first composite 1 and the second composite 2 as shown in FIG. may be correspondingly located or may be located at different locations.
  • a method for manufacturing a joined body according to an embodiment of the present disclosure includes the following steps (a) to (c).
  • Step (a) and step (b) are steps for obtaining the first complex 1 and the second complex 2, respectively.
  • First, 8.7 parts by mass to 42.9 parts by mass of silicon powder having an average particle size of 1 ⁇ m to 90 ⁇ m are mixed with 100 parts by mass of ⁇ -type silicon carbide powder having an average particle size of 40 ⁇ m to 250 ⁇ m. do.
  • a thermosetting resin is added as a molding aid so that the percentage of residual carbon after degreasing treatment is 10% or more.
  • the average particle size of silicon carbide and silicon can be measured by a liquid phase sedimentation method, a light throwing method, a laser scattering diffraction method, or the like.
  • thermosetting resin is not limited, and examples thereof include phenol resin, epoxy resin, furan resin, phenoxy resin, melamine resin, urea resin, aniline resin, unsaturated polyester resin, urethane resin, and methacrylic resin. These resins may be used alone or in combination of two or more. In terms of low shrinkage after thermosetting, it is preferable to use, for example, a resol-type or novolac-type phenolic resin as the molding aid.
  • a powder containing 95% by mass or more of silicon may be used, and a powder containing 99% by mass or more of silicon is preferably used.
  • the shape of the silicon powder to be used is not limited, and may be, for example, spherical, nearly spherical, or irregular.
  • the silicon powder becomes a silicon phase by heat treatment and connects crystal grains of silicon carbide.
  • the mixed raw materials are granulated using a granulator such as a tumbling granulator, spray layer, compression granulator, and extrusion granulator to obtain granules.
  • a tumbling granulator may be used to obtain granules having a large particle size (for example, 0.4 mm or more and 1.6 mm or less).
  • the granulation time is not limited, and 30 minutes or longer is preferable in consideration of the crushability of the compact.
  • the particle size of the granules is not limited, and considering the crushability and handleability of the compact, it is preferably 0.4 mm or more and 1.6 mm or less, and may be 0.5 mm or more and 1.5 mm or less.
  • the obtained granules are molded.
  • methods for molding granules include dry pressure molding and cold isostatic pressing.
  • the pressure during molding is, for example, 78.4 MPa or more and 117.6 MPa or less.
  • a sintered body is obtained by heat-treating the obtained molded body at 1460° C. or higher and 1500° C. or lower in a non-oxidizing atmosphere.
  • a degreasing treatment may be performed at a temperature of 400° C. or higher and 600° C. or lower in a non-oxidizing atmosphere such as argon, helium, neon, or vacuum.
  • FIG. 2 is an explanatory diagram showing steps of a manufacturing method according to an embodiment of the present disclosure.
  • a first recess 13 and a second recess 23 are formed in the sintered body (member) thus obtained.
  • the member is subjected to oxidation treatment to form an oxide film containing silicon oxide as a main component on the surface of the member.
  • This oxide film corresponds to "first outer layer portion 11 and first inner layer portion 14" and “second outer layer portion 21 and second inner layer portion 24", and the remaining portions correspond to "first inner layer portion 12" and "second inner layer portion”. 22”.
  • the thicknesses of “first outer layer portion 11 and first inner layer portion 14” and “second outer layer portion 21 and second inner layer portion 24” are as described above.
  • the first composite 1 and the second composite 2 are obtained.
  • Step (c) is a step of grinding or polishing at least one of the first contact surface 15 of the first composite 1 and the second contact surface 25 of the second composite 2 .
  • Step (c) is a step of grinding or polishing at least one of the first contact surface 15 of the first composite 1 and the second contact surface 25 of the second composite 2 .
  • the method of grinding or polishing is not limited. For example, it is polished by grinding, lapping, polishing, or the like.
  • the step (d) is a step of contacting the first contact surface and the second contact surface and heat-treating them.
  • the heat treatment is performed in a vacuum atmosphere or an inert gas atmosphere.
  • the heat treatment temperature is, for example, 1100° C. or higher and 1650° C. or lower.
  • silicon is moderately melted around each of the first contact surface 15 and the second contact surface 25, and the first composite 1 and the second composite 2 are strengthened.
  • can be joined to By setting the heat treatment temperature to 1650° C. or less, and by not melting anything other than the above-mentioned peripheries, the rigidity of each of the first composite 1 and the second composite 2 can be maintained in a high state.
  • the heat treatment time is appropriately set according to the size of the first composite 1 and the second composite 2, and is, for example, 1 minute or more and 180 minutes or less.
  • the first contact surface 15 and the second contact surface 25 of the first composite 1 and the second composite 2 are diffusion-bonded to obtain the bonded body 10 according to one embodiment.
  • the pressure may be applied from the thickness direction, or only the weight of the upper member may be applied.
  • a joined body according to the present disclosure is used, for example, as a member exposed to a high temperature environment of 500°C or higher, or 800°C or higher, in a heat exchange device.
  • a member includes, for example, a heat exchanger for water and high-temperature gas because of its high strength at high temperatures.
  • Example 1 First, a first composite and a second composite were produced respectively. Before diffusion bonding, the first contact surface of the first composite and the second contact surface of the second composite were brought into the state shown in Table 1 in advance. The first contact surface and the second contact surface were brought into contact with each other, and diffusion bonding was performed at a heat treatment temperature of 1350° C. in a vacuum atmosphere to obtain a sample.
  • the mirror surface obtained by polishing the cross section including the first contact surface and the second contact surface of each sample was observed with a scanning electron microscope at a magnification of 250 times for the presence or absence of voids.
  • the length of the first contact surface (second contact surface) on the mirror surface was set to 0.35 mm, and the void in this length was the object of observation.
  • Samples in which voids with a maximum length in the thickness direction exceeding 20 ⁇ m were observed were rated as “present”, and other samples were rated as “absent”. Table 1 shows the results.
  • sample No. 2 to 4 do not include a gap between the first contact surface and the second contact surface. That is, no voids having a maximum length in the thickness direction exceeding 20 ⁇ m were observed. Therefore, it can be said that good diffusion bonding is obtained.
  • Example 2 First, a sample made of the joined body of the present embodiment was prepared. The contents of silicon carbide and silicon contained in each sample were adjusted in advance to the values shown in Table 2. Each component contained in the first interior and the second interior of each sample was identified with an X-ray diffractometer, and each content of silicon carbide and silicon was obtained by the Rietveld method. Contents of components other than silicon carbide and silicon were found to be 0.1% by mass or less as a result of determination by a fluorescent X-ray spectrometer. Dynamic elastic modulus and thermal conductivity were measured for each sample.
  • the dynamic elastic modulus was measured using the ultrasonic pulse method described in JIS R 1602:1995.
  • the sample used for the measurement of the dynamic elastic modulus is a prism of 10 mm square and 40 mm in length, and the first contact surface and the second contact surface (both rectangular with a length of 40 mm and a width of 10 mm) are the samples. It was arranged so as to be perpendicular to the laser pulse light irradiated to the Table 2 shows the results.
  • Thermal conductivity was measured using the flash method described in JIS R 1611: 2010 (ISO 18755: 2005 (MOD). A plate was arranged so that the first contact surface and the second contact surface (both circular with a diameter of 3 mm) were perpendicular to the laser pulse light irradiated to the sample.
  • the mirror surface obtained by polishing the cross-section including the first contact surface and the second contact surface of each sample was observed for the presence or absence of voids in the same manner as in Example 1. It was confirmed that there were no voids in any of the samples.
  • the content of silicon carbide in at least one of the first interior and the second interior is 70% by mass or more and 92% by mass or less. Therefore, it can be said that it has both a high dynamic elastic modulus and a high thermal conductivity.
  • Example 3 First, a sample made of the joined body of the present embodiment was prepared. The content of silicon carbide contained in each sample was adjusted to 81% by mass, and the content of silicon was adjusted to 19% by mass.
  • Table 3 shows the pressure used in molding to obtain the first interior and the second interior as molding pressure. The mirror surface obtained by polishing the cross section including the first contact surface and the second contact surface of each sample was observed for the presence or absence of voids in the same manner as in Example 1. As a result, all samples had voids. Confirmed not.
  • the distance between the centers of gravity of silicon in the first inner part and the second inner part of each sample was obtained by the following method. First, a sample including the first inner part and the second inner part was separately cut out, and an average range was selected from the mirror surface obtained by polishing the cross section of the sample using diamond abrasive grains. An observation image was obtained by photographing a range of 191 mm 2 (horizontal length: 351 ⁇ m, vertical length: 545 ⁇ m) with a CCD camera.
  • the distance between the centers of gravity of silicon was measured using the image analysis software ⁇ Azo-kun (ver. asked for The setting conditions for this method were a threshold value of 190, which is an index indicating the brightness of the image, a brightness of light, a small figure removal area of 1 ⁇ m 2 , and a noise removal filter.
  • the circle-equivalent diameter of silicon was obtained by a technique called particle analysis, using the observed image as a target.
  • the setting conditions for this method were as follows: the threshold value, which is an index indicating the brightness of the image, was set to 195; the brightness was bright; the small figure removal area was 1 ⁇ m 2 ;
  • the average value of the distance between the centers of gravity of silicon and the average value of the equivalent circle diameter were calculated, and the value obtained by subtracting the average value of the average equivalent circle diameter from the average value of the distance between the centers of gravity of silicon was shown in Table 3 as the silicon spacing.
  • the distance between silicon atoms in at least one of the first interior and the second interior is 8 ⁇ m or more and 20 ⁇ m or less. Therefore, it has both a high dynamic elastic modulus and a high thermal conductivity, and it can be said that there is little bias in rigidity and thermal conductivity.

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Abstract

本開示に係る接合体の製造方法は、外面側に位置し酸化珪素を主成分として含む第１外層部、および第１外層部に囲繞される炭化珪素および珪素を含む第１内部を有する第１複合体を得る工程と；外面側に位置し酸化珪素を主成分として含む第２外層部、および第２外層部に囲繞される炭化珪素および珪素を含む第２内部を有する第２複合体を得る工程と；第１内部が第２内部に当接する第１当接面、および第２内部が第１内部に当接する第２当接面の少なくとも一方を、研削または研磨する工程と；第１当接面と第２当接面とを当接させ、真空雰囲気中または不活性ガス雰囲気中で熱処理する工程とを含む。

Description

接合体の製造方法
　本発明は、接合体の製造方法に関する。
　従来、炭化ケイ素セラミックス材同士の接合は、特許文献１に記載のように、ろう材を用いて行われている。具体的には、特許文献１には、炭化ケイ素セラミックス材同士を、シリコンを含むろう材を用いて接合させる際、炭化ケイ素セラミックス材の非接合面にのみ、予め、酸化膜を形成する方法が記載されている。このような方法によって、炭化ケイ素セラミックス材同士を細孔または溝を有する面で接合させても、細孔または溝が閉塞しないようにしている。
特許第４９５４８３８号公報
　本開示に係る接合体の製造方法は、外面側に位置し酸化珪素を主成分として含む第１外層部、および第１外層部に囲繞される炭化珪素および珪素を含む第１内部を有する第１複合体を得る工程と；外面側に位置し酸化珪素を主成分として含む第２外層部、および第２外層部に囲繞される炭化珪素および珪素を含む第２内部を有する第２複合体を得る工程と；第１内部が第２内部に当接する第１当接面、および第２内部が第１内部に当接する第２当接面の少なくとも一方を、研削または研磨する工程と；第１当接面と第２当接面とを当接させ、真空雰囲気中または不活性ガス雰囲気中で熱処理する工程とを含む。
本開示の一実施形態に係る製造方法によって得られる接合体を示す説明図である。 本開示の一実施形態に係る製造方法の工程を示す説明図である。
　上述のように従来の接合方法は、ろう材を用いているため、炭化ケイ素セラミックス材間にろう材層が存在する。その結果、ろう材層内に空隙が存在すると、接合強度が低下する。このろう材層の厚みのばらつきを抑制するには、シリコンの粒度分布を制御する必要がある。制御が適切にされなければ、外部に流体がリークすることがある。さらに、従来の接合方法では、炭化ケイ素セラミックス材同士を、真空ろう付けによって接合している。そのため、ろう材に含まれる炭素が飛散し、炉壁を汚すことがある。
　したがって、優れた接合強度を有する接合体、および炉壁を汚さずに、優れた接合強度を有する接合体を製造する方法が求められている。
　本開示に係る接合体の製造方法は、上記のように、第１当接面と第２当接面とを当接させ、真空雰囲気中または不活性ガス雰囲気中熱処理する工程とを含む。したがって、本開示によれば、炉壁を汚さずに、優れた接合強度を有する接合体を製造する方法を提供することができる。
　本開示の一実施形態に係る製造方法によって得られる接合体（以下、「一実施形態に係る接合体」と記載する場合がある）は、上記のように、第１複合体および第２複合体を備える。本開示に係る接合体を、図１に基づいて説明する。
　図１に示すように、一実施形態に係る接合体１０は、第１複合体１および第２複合体２を備える。第１複合体１は、第１外層部１１と第１外層部１１に囲繞される第１内部１２とを有する。第１外層部１１は第１複合体１の外面側に位置しており、酸化珪素を主成分として含む。第１外層部１１は酸化珪素を主成分として含む酸化膜であり、その厚みは限定されない。第１外層部１１は、例えば７００ｎｍ以上９００ｎｍ以下の厚みを有する。
　本明細書において「主成分」とは、８０質量％以上を占める成分を意味する。成分の同定は、ＣｕＫα線を用いたＸ線回折装置で行い、炭化珪素および珪素の含有量は、例えば、リートベルト法により求めればよい。
　第１内部１２は炭化珪素および珪素を含み、第１外層部１１に囲繞されている。具体的には、炭化珪素および珪素を含む部材において、この部材の外側面を酸化して形成される酸化珪素を主成分とする酸化膜が「第１外層部１１」に相当し、残りの部分が「第１内部１２」に相当する。
　第１内部１２に含まれる炭化珪素および珪素の含有量は限定されない。炭化珪素は、例えば、７０質量％以上９２質量％以下の割合で含まれていてもよい。炭化珪素は珪素よりもヤング率（動的弾性率）および３点曲げ強度といった機械的特性に優れている。そのため、炭化珪素の含有量が７０質量％以上の場合、得られる接合体の機械的特性が向上する。一方、珪素は炭化珪素よりも熱伝導率が高い。そのため、炭化珪素の含有量が９２質量％以下の場合、得られる接合体の熱伝導性が向上する。したがって、炭化珪素の含有量が７０質量％以上９２質量％以下であれば、機械的特性と熱伝導性とを両立させることができる。
　第１内部１２において、珪素の重心間距離の平均値と珪素の円相当径の平均値との差は限定されず、例えば、８μｍ以上２０μｍ以下であってもよい。この差が８μｍ以上であると、炭化珪素の分布密度が高くなる。そのため、得られる接合体の剛性が向上し、剛性の偏りも低減される。一方、この差が２０μｍ以下であると、得られる接合体の熱伝導性が向上し、熱伝導性の偏りも低減される。
　第１内部１２の閉気孔率は限定されず、例えば、０．１％以下であってもよい。第１内部１２の閉気孔率が０．１％以下であれば、閉気孔の容積が少なくなる。そのため、得られる接合体において、閉気孔にパーティクルが含まれていたとしても、珪素がパーティクルに侵食されるおそれが低減する。
　第２複合体２は、第２外層部２１と第２外層部２１に囲繞される第２内部２２とを有する。第２外層部２１は第２複合体２の外面側に位置しており、酸化珪素を主成分として含む。第２外層部２１は酸化珪素を主成分として含む酸化膜であり、その厚みは限定されない。第２外層部２１は、例えば７００ｎｍ以上９００ｎｍ以下の厚みを有する。「主成分」については上述の通りであり、詳細な説明は省略する。
　第２内部２２は炭化珪素および珪素を含み、第２外層部２１に囲繞されている。具体的には、炭化珪素および珪素を含む部材において、この部材の外側面を酸化して形成される酸化珪素を主成分とする酸化膜が「第２外層部２１」に相当し、残りの部分が「第２内部２２」に相当する。
　第２内部２２に含まれる炭化珪素および珪素の含有量は限定されない。炭化珪素は、例えば、７０質量％以上９２質量％以下の割合で含まれていてもよい。炭化珪素は珪素よりもヤング率（動的弾性率）および３点曲げ強度といった機械的特性に優れている。そのため、炭化珪素の含有量が７０質量％以上の場合、得られる接合体の機械的特性が向上する。一方、珪素は炭化珪素よりも熱伝導率が高い。そのため、炭化珪素の含有量が９２質量％以下の場合、得られる接合体の熱伝導性が向上する。したがって、炭化珪素の含有量が７０質量％以上９２質量％以下であれば、機械的特性と熱伝導性とを両立させることができる。第１内部２１および第２内部２２に含まれる各成分は、Ｘ線回折装置で同定し、炭化珪素および珪素の各含有量は、リートベルト法で求めればよい。
　第２内部２２において、珪素の重心間距離の平均値と珪素の円相当径の平均値との差は限定されず、例えば、８μｍ以上２０μｍ以下であってもよい。この差が８μｍ以上であると、炭化珪素の分布密度が高くなる。そのため、得られる接合体の剛性が向上し、剛性の偏りも低減される。一方、この差が２０μｍ以下であると、得られる接合体の熱伝導性が向上し、熱伝導性の偏りも低減される。
　第１内部２１および第２内部２２における珪素の重心間距離は、以下の方法で求めればよい。まず、第１内部２１および第２内部２２のそれぞれ一部を切り出す。切り出した後、ダイヤモンド砥粒を用い、断面を研磨して得られる鏡面から、平均的な範囲を選択する。その後、各面積が０．１９１ｍｍ2（横方向の長さが３５１μｍ、縦方向の長さが５４５μｍ）となる範囲を走査型電子顕微鏡で撮影して、観察像を得る。
　この観察像を対象として、画像解析ソフト「Ａ像くん(ｖｅｒ２．５２)」（登録商標、旭化成エンジニアリング（株）製、以降の説明において画像解析ソフト「Ａ像くん」と記した場合、旭化成エンジニアリング（株）製の画像解析ソフトを示す）を用いて分散度計測の重心間距離法という手法で珪素の重心間距離を求める。
　この手法の設定条件としては、画像の明暗を示す指標であるしきい値を１９０～１９５、明度を明、小図形除去面積を１μｍ2、雑音除去フィルタを有とする。珪素の円相当径は、上記観察像を対象として、粒子解析という手法で求める。この手法の設定条件は、重心間距離法で用いた設定条件と同じである。
　第２内部２２の閉気孔率は限定されず、例えば、０．１％以下であってもよい。第２内部２２の閉気孔率が０．１％以下であれば、閉気孔の容積が少なくなる。そのため、得られる接合体において、閉気孔にパーティクルが含まれていたとしても、珪素がパーティクルに侵食されるおそれが低減する。珪素の円相当径は、上記観察像を対象として、粒子解析という手法で求めればよい。この手法の設定条件は、画像の明暗を示す指標であるしきい値を１５５、明度を暗、小図形除去面積を１μｍ2、雑音除去フィルタを有とする。
　第１複合体１および第２複合体２が、それぞれ第１外層部１１および第２外層部２１を有することによって、接合体１０が高温条件下に曝されたとしても、第１内部１２および第２内部２２の形状安定性が向上する。その理由は、酸化珪素の融点は珪素の融点よりも高いためである。
　一実施形態に係る接合体１０において、第１内部１２が第２内部２２に当接する第１当接面１５と、第２内部２２が第１内部１２に当接する第２当接面２５とは、拡散接合している。拡散接合とは、接着剤などを介さずに部材同士を接合させることであり、部材同士を密着させて、部材の融点以下の温度条件下で、接合面間に生じる原子の拡散を利用して部材同士を接合することである。一実施形態に係る接合体１０では、第１当接面１５および第２当接面２５において珪素原子（Ｓｉ）が拡散し、接合している。
　一実施形態に係る接合体１０において、第１当接面１５と第２当接面２５との間に空隙が含まれない。第１当接面１５と第２当接面２５とが拡散接合しており、第１当接面１５と第２当接面２５との間に空隙が含まれないため、接合体１０は優れた接合強度を有する。さらに、接合体１０において、第１内部１２と第２内部２２との熱交換が容易に行われる。
　「第１当接面１５と第２当接面２５との間に空隙が含まれない」とは、第１当接面１５と第２当接面２５との間で厚み方向の最大長が２０μｍを超える空隙を含まないことを意味する。そのため、最大長が２０μｍ以下の微細な空隙のみが含まれている場合も、「空隙が含まれない」に相当する。空隙については、例えば、第１当接面１５および第２当接面２５を含む断面を研磨して得られる鏡面を、走査型電子顕微鏡を用いて、２５０倍程度の倍率で観察すればよい。鏡面における第１当接面（第２当接面）の長さを、例えば０．３５ｍｍとして、この長さにおける空隙の最大長を測定すればよい。
　一実施形態に係る接合体１０において、第１当接面１５には、図１に示すように、深さ方向に向かって第１凹部１３が備えられていてもよい。このような第１凹部１３が備えられていることによって、得られる接合体１０の第１凹部１３に流体を流すことができる。流体の速度や粘性に応じて、第１凹部１３の幅や深さは適宜調整することができる。そのため、第１凹部１３におけるフィレットの影響（例えば、フィレットによって生じる流体の乱流の発生）は、無視できるほど低減される。その結果、第１凹部１３に流体を流しても、流路抵抗のばらつきを低減することができる。
　第１凹部１３の大きさおよび形状は限定されず、接合体１０の大きさ、用途、流す流体の種類などに応じて適宜設定すればよい。さらに、第１凹部１３の代わりに貫通孔（第１貫通孔）であってもよい。
　第１凹部１３の内壁面および内底面の少なくとも一方、または第１貫通孔の内壁面には、酸化珪素を主成分として含む第１内層部１４が備えられていてもよい。このような第１内層部１４が備えられていると、上述の第１外層部１１と同様、接合体１０において、第１凹部１３または第１貫通孔が高温条件下に曝されたとしても、第１凹部１３または第１貫通孔の形状安定性が向上する。その理由は、上述の通りであり、酸化珪素の融点は珪素の融点よりも高いためである。第１内層部１４は、例えば７００ｎｍ以上９００ｎｍ以下の厚みを有していてもよい。
　一実施形態に係る接合体１０において、第２当接面２５には、図１に示すように、深さ方向に向かって第２凹部２３が備えられていてもよい。このような第２凹部２３が備えられていることによって、得られる接合体１０の第２凹部２３に流体を流すことができる。第２凹部２３についても、第１凹部１３と同様、第２凹部２３に流体を流しても、流路抵抗のばらつきを低減することができる。
　第２凹部２３の大きさおよび形状は限定されず、接合体１０の大きさ、用途、流す流体の種類などに応じて適宜設定すればよい。さらに、第２凹部２３の代わりに貫通孔（第２貫通孔）であってもよい。
　第２凹部２３の内壁面および内底面の少なくとも一方、または第２貫通孔の内壁面には、酸化珪素を主成分として含む第２内層部２４が備えられていてもよい。理由については、上述の第１凹部１３において説明した通りである。第２内層部２４は、例えば７００ｎｍ以上９００ｎｍ以下の厚みを有していてもよい。
　第１凹部１３（または第１貫通孔）と第２凹部２３（または第１貫通孔）とは、同じ形状であってもよく、異なる形状であってもよい。さらに、第１凹部１３（または第１貫通孔）と第２凹部２３（または第１貫通孔）とは、図１に示すように、第１複合体１と第２複合体２とを接合させた場合に、対応するように位置していてもよく、異なる場所に位置していてもよい。
　本開示の一実施形態に係る接合体の製造方法は、下記の工程（ａ）～（ｃ）を含む。
　　工程（ａ）：外面側に位置し酸化珪素を主成分として含む第１外層部、および第１外層部に囲繞される炭化珪素および珪素を含む第１内部を有する第１複合体を得る工程。
　　工程（ｂ）：外面側に位置し酸化珪素を主成分として含む第２外層部、および第２外層部に囲繞される炭化珪素および珪素を含む第２内部を有する第２複合体を得る工程。
　　工程（ｃ）：第１内部が第２内部に当接する第１当接面、および第２内部が第１内部に当接する第２当接面の少なくとも一方を、研削または研磨する工程。
　　工程（ｄ）：第１当接面と第２当接面とを当接させ、真空雰囲気中または不活性ガス雰囲気中で熱処理する工程。
　工程（ａ）および工程（ｂ）は、それぞれ第１複合体１および第２複合体２を得る工程である。まず、４０μｍ以上２５０μｍ以下の平均粒径を有するα型炭化珪素粉末１００質量部に対して、１μｍ以上９０μｍ以下の平均粒径を有する珪素粉末８．７質量部以上４２．９質量部以下を混合する。得られたα型炭化珪素と珪素との混合粉末に、成形助剤として、脱脂処理後の残炭率が１０％以上となるような熱硬化性樹脂を添加する。炭化珪素および珪素の平均粒径は、液相沈降法、光投下法、レーザー散乱回折法などによって測定することができる。
　熱硬化性樹脂としては、限定されず、例えば、フェノール樹脂、エポキシ樹脂、フラン樹脂、フェノキシ樹脂、メラミン樹脂、尿素樹脂、アニリン樹脂、不飽和ポリエステル樹脂、ウレタン樹脂、メタクリル樹脂などが挙げられる。これらの樹脂は、単独で使用してもよく、２種以上を併用してもよい。熱硬化後の低収縮性の点で、成形助剤としては、例えば、レゾール型またはノボラック型のフェノール樹脂を使用するのがよい。
　珪素粉末の純度については高い方がよい。珪素を９５質量％以上の割合で含む粉末を使用してもよく、珪素を９９質量％以上の割合で含む粉末を使用するのがよい。使用する珪素粉末の形状は限定されず、例えば、球形または球形に近い形状であってもよく、不規則形状であってもよい。珪素粉末は、熱処理によって珪素相となり、炭化珪素の結晶粒子を連結する。
　次いで、混合した原料を、転動造粒機、スプレードレイヤー、圧縮造粒機、押出造粒機などの造粒機を使用して造粒することによって顆粒を得る。大きな粒径（例えば、０．４ｍｍ以上１．６ｍｍ以下）を有する顆粒を得るためには、転動造粒機を使用すればよい。造粒時間は限定されず、成形体の潰れ性を考慮すると、３０分以上造粒するのがよい。顆粒の粒径は限定されず、成形体の潰れ性やハンドリング性を考慮すると、０．４ｍｍ以上１．６ｍｍ以下であるのがよく、０．５ｍｍ以上１．５ｍｍ以下であってもよい。
　次いで、得られた顆粒を成形する。顆粒を成形する方法としては、例えば、乾式加圧成形法、冷間等方静水圧成形法などが挙げられる。成形する際の圧力は、例えば、７８．４ＭＰａ以上１１７．６ＭＰａ以下である。得られた成形体を、非酸化雰囲気下、１４６０℃以上１５００℃以下で熱処理することによって、焼結体が得られる。熱処理する前に、必要に応じて、アルゴン、ヘリウム、ネオン、真空などの非酸化雰囲気下、４００℃以上６００℃以下の温度で脱脂処理を行ってもよい。
　図２は、本開示の一実施形態に係る製造方法の工程を示す説明図である。このようにして得られた焼結体（部材）に第１凹部１３および第２凹部２３を形成する。その後、部材を酸化処理に供して、部材の表面に酸化珪素を主成分とする酸化膜を形成する。この酸化膜が「第１外層部１１および第１内層部１４」ならびに「第２外層部２１および第２内層部２４」に相当し、残りの部分が「第１内部１２」および「第２内部２２」に相当する。「第１外層部１１および第１内層部１４」ならびに「第２外層部２１および第２内層部２４」の厚みは、上述の通りである。このようにして、第１複合体１および第２複合体２が得られる。
　工程（ｃ）は、第１複合体１の第１当接面１５、および第２複合体２の第２当接面２５の少なくとも一方を、研削または研磨する工程である。第１当接面１５および第２当接面２５の少なくとも一方を研削または研磨することによって、接合した際の密着性を向上させることができる。その結果、優れた接合強度が発揮される。接合強度を向上させる点で、第１当接面１５および第２当接面２５の両方を研削または研磨してもよい。
　研削または研磨する方法は限定されない。例えば、研削または、ラップ加工、ポリッシュ加工などによって研磨される。
　工程（ｄ）は、第１当接面と第２当接面とを当接させ、熱処理する工程である。熱処理は、真空雰囲気中または不活性ガス雰囲気中で行われる。熱処理温度は、例えば、１１００℃以上１６５０℃以下である。熱処理温度を１１００℃以上とすることで、第１当接面１５および第２当接面２５の各周辺で珪素が適度に溶融して、第１複合体１と第２複合体２とを強固に接合することができる。熱処理温度を１６５０℃以下とすること、上記各周辺以外を溶融させることがないので、第１複合体１および第２複合体２の各剛性を高い状態で維持することができる。
　不活性ガスとしては、例えば、アルゴン、ヘリウム、ネオンなどが挙げられる。熱処理の時間は、第１複合体１および第２複合体２の大きさなどに応じて適宜設定され、例えば、１分以上１８０分以下である。このようにして、第１複合体１および第２複合体２において、第１当接面１５と第２当接面２５とが拡散接合され、一実施形態に係る接合体１０が得られる。なお、第１当接面１５と第２当接面２５とを当接させ、熱処理する場合、厚み方向から押圧しても、上側に位置する部材の自重のみであってもよい。
　本開示に係る接合体は、例えば、熱交換装置において、５００℃以上、さらには８００℃以上高温環境下に曝されるような部材として使用される。このような部材としては、高温での強度が高いことから、例えば、水と高温のガスとの熱交換器などが挙げられる。
　以下、本発明の実施例を具体的に説明するが、本発明はこれらの実施例により限定されるものではない。
（実施例１）
　まず、第１複合体および第２複合体をそれぞれ作製した。拡散接合する前に、第１複合体の第１当接面および第２複合体の第２当接面とは、予め表１に示す状態の面になるようにした。第１当接面と第２当接面とを当接させ、真空雰囲気中で熱処理温度を１３５０℃として拡散接合して試料を得た。
　各試料の第１当接面および第２当接面を含む断面を研磨して得られる鏡面を、走査型電子顕微鏡を用いて、２５０倍の倍率で、空隙の有無を観察した。ここで、鏡面における第１当接面（第２当接面）の長さを０．３５ｍｍとし、この長さにおける空隙を観察の対象とした。厚み方向の最大長が２０μｍを超える空隙が観察された試料は、「有」、それ以外の試料については「無」とし、その結果を表１に示す。
Figure JPOXMLDOC01-appb-T000001
　表１に示すように、試料Ｎｏ．２～４は、第１当接面と第２当接面との間に空隙が含まれていない。すなわち、厚み方向の最大長が２０μｍを超える空隙が観察されていない。そのため、良好な拡散接合が得られていると言える。
（実施例２）
　まず、本実施形態の接合体からなる試料を準備した。各試料に含まれる炭化珪素および珪素の各含有量は、予め表２に示す値になるように調整した。各試料の第１内部および第２内部に含まれる各成分は、Ｘ線回折装置で同定し、炭化珪素および珪素の各含有量は、リートベルト法で求めた。炭化珪素および珪素以外の成分の含有量は、蛍光Ｘ線分析装置で求めた結果、その含有量の合計は０．１質量％以下であった。各試料について、動的弾性率および熱伝導率を測定した。
　動的弾性率は、ＪＩＳ　Ｒ　１６０２：１９９５に記載された超音波パルス法を用いて測定した。動的弾性率の測定に用いる試料は、１０ｍｍ角、長さが４０ｍｍの角柱であり、第１当接面および第２当接面（いずれも長さが４０ｍｍ、幅が１０ｍｍの矩形）が試料に照射するレーザーパルス光に対して垂直になるように配置した。結果を表２に示す。
　熱伝導率は、ＪＩＳ　Ｒ　１６１１：２０１０（ＩＳＯ　１８７５５：２００５（ＭＯＤ）に記載されたフラッシュ法を用いて測定した。熱伝導率の測定に用いる試料は、直径が１０ｍｍ、厚さが３ｍｍの円板とし、第１当接面および第２当接面（いずれも直径が３ｍｍの円形）が試料に照射するレーザーパルス光に対して垂直になるように配置した。結果を表２に示す。
　各試料の第１当接面および第２当接面を含む断面を研磨して得られる鏡面を実施例１で示した方法と同じ方法で空隙の有無を観察した。いずれの試料も空隙がないことを確認した。
Figure JPOXMLDOC01-appb-T000002
　表２に示すように、試料Ｎｏ．６～１９は、第１内部および第２内部の少なくともいずれかにおける炭化珪素の含有量が７０質量％以上９２質量％以下である。そのため、高い動的弾性率と高い熱伝導率とを兼ね備えていると言える。
（実施例３）
　まず、本実施形態の接合体からなる試料を準備した。各試料に含まれる炭化珪素の含有量は８１質量％、珪素の含有量は１９質量％になるように調整した。ここで、第１内部および第２内部を得るために、成形する際に用いる圧力を成形圧として表３に示した。各試料の第１当接面および第２当接面を含む断面を研磨して得られる鏡面を実施例１で示した方法と同じ方法で空隙の有無を観察した結果、いずれの試料も空隙がないことを確認した。
　各試料の動的弾性率、３点曲げ強度および熱伝導率を実施例１で示した方法と同じ方法で測定した。結果を表３に示した。
　各試料の第１内部および第２内部の珪素の重心間距離は、以下の方法で求めた。まず、第１内部、第２内部を含む試料を別々に切り出して、ダイヤモンド砥粒を用いて試料の断面を研磨して得られる鏡面から、平均的な範囲を選択して、各面積が０．１９１ｍｍ2（横方向の長さが３５１μｍ、縦方向の長さが５４５μｍ）となる範囲をＣＣＤカメラで撮影して、観察像を得た。
　この観察像を対象として、画像解析ソフト「Ａ像くん(ｖｅｒ２．５２)」（登録商標、旭化成エンジニアリング（株）製）を用いて分散度計測の重心間距離法という手法で珪素の重心間距離を求めた。この手法の設定条件としては、画像の明暗を示す指標であるしきい値を１９０、明度を明、小図形除去面積を１μｍ2、雑音除去フィルタを有とした。
　珪素の円相当径は、上記観察像を対象として、粒子解析という手法で求めた。この手法の設定条件としては、画像の明暗を示す指標であるしきい値を１９５とした以外は、明度を明、小図形除去面積を１μｍ2、雑音除去フィルタを有とした。珪素の重心間距離および円相当径の平均値をそれぞれ算出し、珪素の重心間距離の平均値から円相当径の平均値を引いた値を珪素の間隔として表３に示した。
Figure JPOXMLDOC01-appb-T000003
　表３に示すように、試料Ｎｏ．２２～３５は、第１内部および第２内部の少なくともいずれかにおける珪素の間隔が８μｍ以上２０μｍ以下である。そのため、高い動的弾性率と高い熱伝導率とを兼ね備えており、剛性および熱伝導性に偏りが少ないと言える。
　１０　接合体
　１　　第１複合体
　１１　第１外層部
　１２　第１内部
　１３　第１凹部
　１４　第１内層部
　１５　第１当接面
　２　　第２複合体
　２１　第２外層部
　２２　第２内部
　２３　第２凹部
　２４　第２内層部
　２５　第２当接面

Claims (8)

  1. 　外面側に位置し酸化珪素を主成分として含む第１外層部、および該第１外層部に囲繞される炭化珪素および珪素を含む第１内部を有する第１複合体を得る工程と、
    　外面側に位置し酸化珪素を主成分として含む第２外層部、および該第２外層部に囲繞される炭化珪素および珪素を含む第２内部を有する第２複合体を得る工程と、
    　前記第１内部が前記第２内部に当接する第１当接面、および前記第２内部が前記第１内部に当接する第２当接面の少なくとも一方を、研削または研磨する工程と、
    　前記第１当接面と前記第２当接面とを当接させ、真空雰囲気中または不活性ガス雰囲気中で熱処理する工程と、
    を含む、接合体の製造方法。
  2. 　前記第１当接面が、深さ方向に向かって第１凹部または第１貫通孔を備える、請求項１に記載の接合体の製造方法。
  3. 　前記第１複合体が、前記第１凹部の内壁面および内底面の少なくとも一方、または前記第１貫通孔の内壁面に、酸化珪素を主成分として含む第１内層部を備える、請求項２に記載の接合体の製造方法。
  4. 　前記第２当接面が、深さ方向に向かって第２凹部または第２貫通孔を備える、請求項１～３のいずれかに記載の接合体の製造方法。
  5. 　前記第２複合体が、前記第２凹部の内壁面および内底面の少なくとも一方、または前記第２貫通孔の内壁面に、酸化珪素を主成分として含む第２内層部を備える、請求項４に記載の接合体の製造方法。
  6. 　前記第１内部および前記第２内部の少なくとも一方における炭化珪素の含有量が、７０質量％以上９２質量％以下である、請求項１～５のいずれかに記載の接合体の製造方法。
  7. 　前記第１内部および前記第２内部の少なくとも一方において、珪素の重心間距離の平均値と珪素の円相当径の平均値との差が、８μｍ以上２０μｍ以下である、請求項１～６のいずれかに記載の接合体の製造方法。
  8. 　前記第１内部および前記第２内部の少なくとも一方の閉気孔率が、０．１％以下である、請求項１～７のいずれかに記載の接合体の製造方法。
PCT/JP2022/014812 2021-03-29 2022-03-28 接合体の製造方法 Ceased WO2022210470A1 (ja)

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