WO2025192594A1 - Structure en céramique - Google Patents

Structure en céramique

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Publication number
WO2025192594A1
WO2025192594A1 PCT/JP2025/009100 JP2025009100W WO2025192594A1 WO 2025192594 A1 WO2025192594 A1 WO 2025192594A1 JP 2025009100 W JP2025009100 W JP 2025009100W WO 2025192594 A1 WO2025192594 A1 WO 2025192594A1
Authority
WO
WIPO (PCT)
Prior art keywords
layer
ceramic structure
void
crystal particles
thickness direction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2025/009100
Other languages
English (en)
Japanese (ja)
Inventor
康平 嶋
真美 飯田
圭太 久保
諭史 豊田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kyocera Corp
Original Assignee
Kyocera Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Kyocera Corp filed Critical Kyocera Corp
Publication of WO2025192594A1 publication Critical patent/WO2025192594A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
    • 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
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/38—Borides

Definitions

  • the disclosed embodiments relate to ceramic structures.
  • Patent Document 1 ceramic structures having thin films formed by chemical vapor deposition (CVD) are known.
  • Patent Document 2 describes that films formed by chemical vapor deposition are dense, void-free, and highly smooth.
  • Patent Document 3 also describes that the pore content should be less than 3% by area.
  • a ceramic structure has a first layer having first crystal particles and a second layer located on the first layer and having second crystal particles.
  • the first crystal particles and the second crystal particles each contain one or more metal elements selected from Al, Si, Ti, Cr, Zr, and Y, and one or more non-metallic elements selected from N, C, and B.
  • the first crystal particles and the second crystal particles are the same compound.
  • the ratio of the diffraction intensity of the (002) plane to the sum of the diffraction intensities of the (002) plane and the (100) plane of the second layer is defined as C1, and C1 is less than 20%.
  • FIG. 1 is a cross-sectional view showing an example of a ceramic structure according to an embodiment.
  • FIG. 2 is an enlarged view of area A shown in FIG.
  • FIG. 3 is a cross-sectional view showing another example of the ceramic structure according to the embodiment.
  • FIG. 4 is a cross-sectional view showing another example of the ceramic structure according to the embodiment.
  • FIG. 5 is a cross-sectional view showing another example of the ceramic structure according to the embodiment.
  • FIG. 6 is a cross-sectional view showing another example of the ceramic structure according to the embodiment.
  • FIG. 7 is an enlarged view of region B shown in FIG.
  • FIG. 8 is a cross-sectional view showing an example of a dendritic structure.
  • FIG. 9 is a flowchart showing an example of a method for manufacturing a ceramic structure according to an embodiment.
  • the above structure leaves room for further improvement in terms of improving the durability of the ceramic structure.
  • Fig. 1 is a cross-sectional view showing an example of a ceramic structure according to an embodiment.
  • the ceramic structure 1 has a first layer 10 and a second layer 20.
  • the first layer 10 has first crystal grains 11.
  • the second layer 20 has second crystal grains 21.
  • the first crystal grains 11 and the second crystal grains 21 each contain one or more metal elements selected from Al, Si, Ti, Cr, Zr, and Y, and one or more non-metal elements selected from N, C, and B.
  • the first layer 10 may contain 50% or more by area of first crystal particles 11.
  • the first layer 10 may contain 80% or more by area of first crystal particles 11.
  • the first layer 10 may contain 90% or more by area of first crystal particles 11.
  • the second layer 20 may contain 50 area% or more of the second crystal particles 21.
  • the second layer 20 may contain 80 area% or more of the second crystal particles 21.
  • the second layer 20 may contain 90 area% or more of the second crystal particles 21.
  • the amount of the second crystal particles 21 contained in the second layer 20 may be greater than the amount of the first crystal particles 11 contained in the first layer 10.
  • the first crystal particles 11 and the second crystal particles 21 are the same compound.
  • the first crystal particles 11 and the second crystal particles 21 may be any of AlN, Si 3 N 4 , SiC, TiN, TiC, ZrN, ZrB, and YN.
  • the first crystal particles 11 may be AlN.
  • Being the same compound means, for example, in the case of AlN, that Al and N are the main components and that the compound can be identified as AlN by XRD.
  • the Al and N do not have to be contained in a 1:1 ratio.
  • the Al content may differ between the first crystal particles 11 and the second crystal particles 21.
  • C1 is the ratio of the diffraction intensity of the (002) plane to the sum of the diffraction intensities of the (002) plane and the (100) plane in X-ray diffraction from the second surface 202, which serves as the surface layer of the second layer 20 located away from the first layer 10, then C1 is less than 20%. In other words, C1 being less than 20% means that the second layer 20 is not C-axis oriented. With this configuration, a second layer 20 with high hardness can be obtained, and a ceramic structure 1 with excellent durability can be provided. C1 may be less than 10%. C1 may be less than 5%.
  • the diffraction intensity used to calculate C1 can be measured using the following method. It can be measured using a Spectris X'Pert PRO MRD X-ray diffraction instrument, with a diffraction angle range (2 ⁇ ) of 10° to 100°.
  • Crystalline phases and diffraction intensities can be measured using the following method.
  • Low-angle incidence measurements are performed using a thin-film X-ray diffractometer, PANalytical's X'Pert PRO-MRD (DY1878).
  • the optical system is configured as follows: X-ray mirror (automatic insertion attenuation plate, mask 5, Soller slit 0.02 rad, slit 1/8), flat-plate collimator, tube: CuK ⁇ , X-rays: 45 kV, 40 mA, 2 ⁇ scan: 10° to 100°, incident angle: 0.1°, step: 0.02°, time: 4.0 seconds/step.
  • whether the crystal grains are AlN can be determined based on JCPDS No. 00-025-1133.
  • the hardness of the second layer 20 may be measured using the nanoindentation method. For example, it may be measured using a HYSITRON TI980 manufactured by Bruker Japan. The measurement temperature may be room temperature.
  • the first layer 10 is a substrate and may have, for example, a substantially circular plate shape.
  • the second layer 20 is located on the substrate (first layer 10), and the second layer 20 may be in contact with the substrate (first layer 10).
  • the substrate contains, for example, a ceramic such as aluminum nitride (AlN) as a main component.
  • the first layer 10 may also contain, for example, aluminum oxide (Al 2 O 3 ), yttria (Y 2 O 3 ), or the like.
  • the first layer 10 may also be a sintered body obtained by firing a raw material powder. When the first layer 10 is a sintered body, the first crystal grains 11 have a high degree of crystallinity. With such a configuration, a ceramic structure with excellent durability can be provided.
  • first crystal particles 11 and the second crystal particles 21 may be hexagonal.
  • the crystals are anisotropic, and by utilizing this anisotropy, it is possible to provide a ceramic structure with excellent durability.
  • first crystal particles 11 and the second crystal particles 21 may be AlN.
  • the second layer 20 may have a void 22 located inside the second layer 20.
  • the void 22 may be long in the thickness direction of the second layer 20 and may be closed at both ends in the thickness direction.
  • the void 22 may have at least one of a first void 22a, one end of which in the thickness direction is in contact with the first layer 10, and a second void 22b, one end of which is separated from the first layer 10. This configuration can reduce residual stress inside the second layer 20, for example. This makes it less likely that delamination or cracks will occur between the first layer 10 and the second layer 20, improving the durability of the ceramic structure 1.
  • the voids 22 may have a vertically elongated shape that is longer in the thickness direction than in the width direction of the second layer 20.
  • the voids 22 may be closed at both ends in the thickness direction of the second layer 20. That is, the voids 22 are located between the first surface 201 of the second layer 20 facing the first layer 10 and the second surface 202 opposite the first surface 201, and may not be exposed to the second surface 202, which is the interface with the outside. Therefore, the second layer 20 has the desired durability even if it has voids 22 inside.
  • the voids 22 are not lattice defects or so-called nanovoids that may exist in the second crystal particles 21.
  • the width of the voids 22 may be, for example, 0.01 ⁇ m or more.
  • the width of the voids 22 may be, for example, 0.05 ⁇ m or more.
  • the width of the voids 22 may be, for example, 1 ⁇ m or less.
  • the width of the voids 22 may be, for example, 0.5 ⁇ m or less.
  • the length of the void 22 may be, for example, 0.2 ⁇ m or more.
  • the length of the void 22 may be, for example, 0.5 ⁇ m or more.
  • the length of the void 22 may be, for example, 5 ⁇ m or less.
  • the length of the void 22 may be, for example, 1 ⁇ m or less.
  • the presence or absence of voids 22 can be confirmed, for example, by observation using an electron microscope.
  • the area ratio of voids 22 to the second layer 20 may be, for example, 3 area% or more.
  • the area ratio of voids 22 may be, for example, 4 area% or more.
  • the area ratio of voids 22 may be, for example, 5 area% or less.
  • the area ratio of voids 22 to the second layer 20 may be measured, for example, at the center of the cross section of the second layer 20 after mirror polishing.
  • Observation using an electron microscope may be performed at a magnification of 1,000x to 50,000x.
  • the electron microscope may be, for example, a JSM7900F manufactured by JEOL Ltd., and may be performed at an accelerating voltage of 5.0 kV.
  • the area ratio of voids 22 may be calculated based on SEM photographs using image analysis software IMAGE Pro 10 manufactured by MEDIA CYBERNETICS.
  • the SEM photograph may be binarized using the Ward method, and the calculation may be performed using the binarized image.
  • the void 22 may have a first void 22a and a second void 22b.
  • the first void 22a is a void 22 whose lower end, which is one end in the thickness direction of the second layer 20, contacts the surface 101 of the first layer 10.
  • the second void 22b is a void 22 whose one end is away from the surface 101 of the first layer 10.
  • the second layer 20 may have both the first void 22a and the second void 22b inside.
  • the second layer 20 may have only one of the first void 22a and the second void 22b.
  • Figure 2 is an enlarged view of area A shown in Figure 1.
  • the second crystal particles 21 in the second layer 20 may have columnar crystals 21a.
  • the columnar crystals 21a may extend, for example, in a direction intersecting the surface 101 of the first layer 10. That is, the columnar crystals 21a may extend in the thickness direction of the second layer 20.
  • the second layer 20 may have a plurality of columnar crystals 21a aligned along the surface 101 of the first layer 10.
  • the width of the voids 22, i.e., the length of the voids 22 in the direction along the surface 101 of the first layer 10, may be smaller at the second end 222 away from the first layer 10 than at the first end 221 in the thickness direction located on the first layer 10 side. This makes it less likely that the voids 22 will crack and spread from the second end 222 toward the second surface 202. This improves the durability of the ceramic structure 1 including the second layer 20.
  • the voids 22 may be located between adjacent columnar crystals 21a. Such voids 22 may be larger or smaller than the columnar crystals 21a.
  • a space 40 may be present between the first layer 10 and the second layer 20.
  • the space 40 refers to a space extending along the surface 101 of the first layer 10. More specifically, in a cross-sectional view, the length of an imaginary line connecting both ends of the space 40 in the direction along the surface 101 is longer than the maximum height of the space 40 in the direction intersecting with the surface 101. More specifically, the length of an imaginary line connecting both ends of the space 40 in the direction along the surface 101 is at least five times, and preferably at least ten times, the height of the space 40 in the direction intersecting with the surface 101.
  • the second layer 20 may have a first portion, which is closer to the first layer 10, having a higher porosity than a second portion, which is farther from the first layer 10 than the first portion. This allows the thermal conductivity of the first portion to be smaller than that of the second portion. Therefore, when a thermal shock is applied to the ceramic structure 1 from the second layer 20 side, a sudden change in the temperature difference that occurs between the first layer 10 and the second layer 20 is suppressed. As a result, the durability of the ceramic structure 1 against thermal shock is improved.
  • the first portion may be, for example, a region including the first surface 201 in the SEM image described above
  • the second portion may be, for example, a region including the second surface 202 in the SEM image described above.
  • the first and second portions may also partially overlap.
  • FIGS. 3 to 5 are cross-sectional views showing another example of a ceramic structure according to an embodiment.
  • the second layer 20 may have a plurality of columnar crystals 21a inclined with respect to the surface 101 of the first layer 10.
  • voids 22 may be located between adjacent columnar crystals 21a. In this way, when the tips of the columnar crystals 21a come into contact with the voids 22, the residual stress of the columnar crystals 21a is reduced, thereby improving the durability of the second layer 20.
  • FIG. 3 illustrates first voids 22a as an example of voids 22, second voids 22b may also be used.
  • the first layer 10 may have unevenness on the surface 101 facing the second layer 20.
  • the first end 221 of the void 22, which is one end in the thickness direction, may be located within the recess 101b of the first layer 10. This prevents the void 22 from spreading in the direction along the surface 101 of the first layer 10 at the first end 221. As a result, the generation of cracks in the columnar crystals 21a adjacent to the first end 221 is suppressed, improving the durability of the ceramic structure 1.
  • the void 22 is located on the convex portion 101a of the first layer 10. Note that while FIG. 4 illustrates the first void 22a as an example of the void 22, the second void 22b may also be used.
  • the void 22 may be located on the convex portion 101a of the first layer 10. Furthermore, although an example in which multiple columnar crystals 21a extend along the thickness direction of the second layer 20 has been described in Figure 4, they may extend at an angle relative to the thickness direction of the second layer 20 to correspond to the irregularities on the surface 101 of the first layer 10.
  • the volume resistivity of the second layer 20 at 25°C may be higher than the volume resistivity of the first layer 10 at 25°C.
  • the volume resistivity of the second layer 20 at 500°C may be higher than the volume resistivity of the first layer 10 at 500°C.
  • the volume resistivity of the second layer 20 at 25°C may be 1 ⁇ 10 12 ⁇ m or more.
  • the volume resistivity of the second layer 20 at 500°C may be 1 ⁇ 10 5 ⁇ m or more.
  • the volume resistivity of the second layer 20 and the first layer 10 may be measured using the three-terminal method in accordance with JIS C 2141:1992.
  • the ceramic structure 1 may have a conductive layer inside.
  • the conductive layer may have a heater function.
  • the conductive layer may also have an adsorption function.
  • the conductive layer may contain, for example, a metal such as W, Mo, Ni, or Pt.
  • the ceramic structure 1 may further include a third layer 30 located between the first layer 10 and the second layer 20.
  • the third layer 30 contains third crystal particles 31, which are the same compound as the second layer 20.
  • the third layer 30 may have the third crystal particles 31 as its main component.
  • the third layer 30 may contain 50 area% or more of the third crystal particles 31.
  • the third layer 30 may contain 80 area% or more of the third crystal particles 31.
  • the third layer 30 may contain 90 area% or more of the third crystal particles 31.
  • Figure 6 is a cross-sectional view showing another example of a ceramic structure according to an embodiment.
  • Figure 7 is an enlarged view of region B shown in Figure 6.
  • the second crystal particles 21 in the second layer 20 may have a dendritic structure 210.
  • the dendritic structure 210 may have a stem 210a and branch portions 210b.
  • the second crystal particles 21 are arranged, for example, in a direction intersecting the surface 101 of the first layer 10 (see FIG. 6). That is, in the stem 210a, the second crystal particles 21 are arranged in the thickness direction of the second layer 20.
  • the second crystal particles 21 may be arranged in a direction perpendicular to the surface 101 of the first layer 10.
  • the stem 210a may include a stem 210c in which the second crystal particles 21 are arranged so as to be tilted from the thickness direction of the first layer 10.
  • the second layer 20 may have multiple trunk portions 210a lined up along the surface 101 of the first layer 10. This configuration improves the thermal conductivity of the second layer 20 in the thickness direction. As a result, the second layer 20 has reduced temperature variation in the thickness direction and improved durability.
  • the second layer 20 may have branch portions 210b in which the second crystal particles 21 are aligned in a direction that has a different crystal structure from the stem portion 210a.
  • This configuration can, for example, reduce residual stress within the second layer 20. This reduces the likelihood of delamination or cracks occurring between the first layer 10 and the second layer 20, improving the durability of the ceramic structure 1.
  • the second layer 20 may have a plurality of first regions 20a aligned along the surface 101 of the first layer 10, and second regions 20b located between adjacent first regions 20a.
  • the trunk portion 210a may be located in the first region 20a.
  • the plurality of branch portions 210b may be located in the second region 20b.
  • FIG 8 is a cross-sectional view showing an example of a dendritic structure.
  • the dendritic structure 210 has a stem portion 210a and a crystal structure different from that of the stem portion 210a.
  • the stem portion 210a has side surfaces 23 and 24 located at both ends in the width direction that intersects with the length direction.
  • the dendritic structure 210 may have branch-like portions 210b as a crystal structure different from the stem-like portion 210a.
  • the branch-like portions 210b may have multiple branch-like portions 210b1 located on the side surface 23 side of the stem-like portion 210a.
  • the branch-like portions 210b may have multiple branch-like portions 210b2 located on the side surface 24 side of the stem-like portion 210a.
  • the dendritic structure 210 may have branch-like portions 210b in which the second crystal particles 21 are arranged at an angle ⁇ of 30° or more and 60° or less relative to the stem-like portion 210a.
  • the trunk portion 210a may be positioned so as to contact the first surface 201 (see Figure 6) of the second layer 20 facing the first layer 10.
  • the trunk portion 210a may be positioned so as to contact the second surface 202 (see Figure 6) opposite the first surface 201.
  • the trunk portion 210a may also be positioned away from the first surface 201 and the second surface 202.
  • branch portion 210b may be in contact with the trunk portion 210a.
  • the branch portion 210b may also be positioned away from the trunk portion 210a.
  • the dendritic structure 210 may have voids 25 where the stem portions 210a and branch portions 210b are not located. This configuration, for example, further reduces residual stress within the second layer 20. As a result, delamination and cracks between the first layer 10 and the second layer 20 are less likely to occur, improving the durability of the ceramic structure 1.
  • the second layer 20 of the ceramic structure 1 may have, as the second crystal particles 21, either or both of columnar crystals 21a and dendritic structures 210.
  • Fig. 9 is a flowchart showing an example of a method for manufacturing a ceramic structure according to an embodiment.
  • a disk-shaped sintered body containing 90% to 99.9% AlN by mass is prepared as the substrate (first layer 10). Then, a second layer containing AlN as its main component is formed on the surface of this substrate using the following procedure.
  • a catalyst is applied to the first gas (step S11).
  • the first gas may contain nitrogen, and ammonia, for example, can be used. Tungsten, for example, can be used as the catalyst.
  • the catalyst is applied to the first gas in an environment of, for example, approximately 1600°C to 2200°C, the first gas is decomposed by the catalytic action, generating multiple active species.
  • step S11 the activated species generated in step S11 and a second gas are supplied to the first layer 10 (step S12).
  • a second gas for example, trimethylaluminum can be used as the second gas.
  • the second layer 20 is formed on the first layer 10 (step S13).
  • the first layer 10 may be heated as necessary.
  • the temperature of the first layer 10 may be set to, for example, 420°C to 1000°C, particularly 600°C to 700°C.
  • the deposition time may be, for example, 0.5 hours to 20 hours depending on the desired thickness.
  • the pressure during deposition of the second layer 20 (deposition pressure) may be 1 Pa to 100 Pa.
  • a ceramic structure 1 may be obtained having a second layer 20 on the first layer 10, the second layer 20 having a different crystal structure depending on the temperature set during deposition (deposition temperature), etc.
  • AlN sintered body containing 98% AlN crystals by mass as the main phase was prepared.
  • This AlN sintered body was processed into a first layer measuring 100 mm square.
  • a conductive layer containing W as the metal was disposed inside the AlN sintered body.
  • This conductive layer was formed into a heater pattern.
  • a second layer was then formed on one surface of the first layer using ammonia as the first gas, trimethylaluminum as the second gas, and tungsten as the catalyst.
  • the deposition temperature and deposition pressure in step S13 are shown in Table 1.
  • the diffraction intensities of the (002) and (100) planes of the second layer of the resulting ceramic structure are shown in Table 1.
  • the ratio of the diffraction intensity of the (002) plane to the sum of the diffraction intensities of the (002) and (100) planes of the second layer is also shown in Table 1 as C1. Blanks or "-" in the table indicate unmeasured or uncalculated data.
  • the surface hardness of the second layer was measured at room temperature using nanoindentation. Hardness was measured using a HYSITRON TI980 manufactured by Bruker Japan. The indentation load of the diamond indenter was adjusted appropriately depending on the thickness of the second layer.
  • Table 1 also lists a sample in which the portions corresponding to the first and second layers were made from a sintered body. Table 1 lists the film formation temperature and the above-mentioned measured values.
  • C1 for sample No. 1 was approximately 37%.
  • C1 for samples No. 2 to 7 was less than 20%.
  • Samples with a small C1 tend to have low hardness, and the hardness of samples No. 4 and 5 was higher than that of sample No. 1, demonstrating excellent durability.
  • a ceramic structure includes a first layer having first crystalline grains; a second layer located on the first layer and having second crystal particles;
  • the first crystal particles and the second crystal particles each include one or more metal elements selected from Al, Si, Ti, Cr, Zr, and Y; and one or more nonmetallic elements selected from N, C, and B, the first crystal particles and the second crystal particles are the same compound;
  • the ratio of the diffraction intensity of the (002) plane to the total diffraction intensity of the (002) plane and the (100) plane of the second layer is defined as C1, The C1 is less than 20%.
  • C1 may be less than 10%.
  • the second layer has a void located therein, the void being elongated in a thickness direction of the second layer, and both ends of the void in the thickness direction being closed;
  • the void may include at least one of a first void having one end in the thickness direction in contact with the first layer and a second void having one end separated from the first layer.
  • the second layer may have a porosity of 3 area % or more and 5 area % or less in a cross section parallel to the thickness direction.
  • the second layer has a plurality of columnar crystals inclined with respect to the surface of the first layer, The voids may be located between adjacent ones of the plurality of columnar crystals.
  • the first layer has irregularities on a surface facing the second layer, One end of the void in the thickness direction may be located within the recess of the first layer.
  • the length of the void in the direction along the surface of the first layer may be smaller at a second end portion away from the first layer than at a first end portion in the thickness direction located on the first layer side.
  • the second layer may have a first portion closer to the first layer that has a greater porosity than a second portion that is farther from the first layer than the first portion.
  • Any one of the ceramic structures (1) to (8) above may have an internal conductive layer.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Products (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

Cette structure en céramique comprend : une première couche ayant des premiers grains cristallins ; et une seconde couche positionnée sur la première couche et ayant des seconds grains cristallins. Les premiers grains cristallins et les seconds grains cristallins contiennent chacun : au moins un élément métallique choisi parmi Al, Si, Ti, Cr, Zr et Y ; et au moins un élément non métallique choisi parmi N, C et B. Les premiers grains cristallins et les seconds grains cristallins sont le même composé. Lorsque la proportion de l'intensité de diffraction du plan (002) par rapport au total des intensités de diffraction du plan (002) et du plan (100) de la seconde couche en diffraction des rayons X à partir d'une couche de surface de la seconde couche positionnée à l'opposé de la première couche est C1, C1 est inférieur à 20 %.
PCT/JP2025/009100 2024-03-13 2025-03-11 Structure en céramique Pending WO2025192594A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04114971A (ja) * 1990-09-05 1992-04-15 Nippon Pillar Packing Co Ltd 複合材
JPH07180057A (ja) * 1993-12-22 1995-07-18 Kyocera Corp 被覆部材
JPH1154603A (ja) * 1997-08-06 1999-02-26 Ngk Insulators Ltd 半導体支持装置
WO2019189378A1 (fr) * 2018-03-27 2019-10-03 日本碍子株式会社 Feuille de nitrure d'aluminium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04114971A (ja) * 1990-09-05 1992-04-15 Nippon Pillar Packing Co Ltd 複合材
JPH07180057A (ja) * 1993-12-22 1995-07-18 Kyocera Corp 被覆部材
JPH1154603A (ja) * 1997-08-06 1999-02-26 Ngk Insulators Ltd 半導体支持装置
WO2019189378A1 (fr) * 2018-03-27 2019-10-03 日本碍子株式会社 Feuille de nitrure d'aluminium

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