WO2022186344A1 - ヒータ - Google Patents
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- WO2022186344A1 WO2022186344A1 PCT/JP2022/009188 JP2022009188W WO2022186344A1 WO 2022186344 A1 WO2022186344 A1 WO 2022186344A1 JP 2022009188 W JP2022009188 W JP 2022009188W WO 2022186344 A1 WO2022186344 A1 WO 2022186344A1
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- WIPO (PCT)
- Prior art keywords
- region
- grain boundary
- heater
- boundary phase
- crystal grains
- Prior art date
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- 239000013078 crystal Substances 0.000 claims abstract description 92
- 239000000919 ceramic Substances 0.000 claims abstract description 66
- 239000000758 substrate Substances 0.000 claims abstract description 51
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 21
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims description 57
- 239000004020 conductor Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 abstract description 42
- 239000012212 insulator Substances 0.000 description 35
- 238000004458 analytical method Methods 0.000 description 7
- 230000035882 stress Effects 0.000 description 7
- 229910052691 Erbium Inorganic materials 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910003564 SiAlON Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/40—Heating elements having the shape of rods or tubes
- H05B3/42—Heating elements having the shape of rods or tubes non-flexible
- H05B3/48—Heating elements having the shape of rods or tubes non-flexible heating conductor embedded in insulating material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/02—Details
- H05B3/06—Heater elements structurally combined with coupling elements or holders
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
- H05B2203/027—Heaters specially adapted for glow plug igniters
Definitions
- the disclosed embodiments relate to heaters.
- a heater includes a ceramic substrate and a heating resistor.
- the ceramic substrate has a plurality of crystal grains made of silicon nitride and a first grain boundary phase located between the plurality of crystal grains and containing an oxide of a rare earth element and silicon.
- a heating resistor is positioned inside the ceramic base.
- the ceramic substrate has a first region including an interface with the heat generating resistor and a second region farther from the heat generating resistor than the first region. The first region has a larger distribution amount of the first grain boundary phase than the second region.
- FIG. 1 is a cross-sectional view showing an example of a heater according to an embodiment.
- FIG. 2 is an enlarged view of area A shown in FIG.
- FIG. 1 is a cross-sectional view showing an example of a heater according to an embodiment.
- the heater 1 according to the embodiment includes a ceramic base 10 and a heat generating resistor 20.
- FIG. 1 is a cross-sectional view showing an example of a heater according to an embodiment.
- the heater 1 according to the embodiment includes a ceramic base 10 and a heat generating resistor 20.
- FIG. 1 is a cross-sectional view showing an example of a heater according to an embodiment.
- the heater 1 according to the embodiment includes a ceramic base 10 and a heat generating resistor 20.
- the heater 1 has, for example, a cylindrical shape.
- the length of the heater 1 can be, for example, about 1 mm to 200 mm, particularly about 20 mm to 60 mm.
- the outer dimension of the heater 1 can be, for example, about 0.5 mm to 100 mm, particularly about 2.5 to 5.5 mm.
- Such a heater 1 is used, for example, as a glow plug, an in-vehicle heater, an automatic soldering apparatus, and other heat sources.
- the heater 1 is not limited to a columnar shape, and may be, for example, an elliptical columnar shape or a prismatic shape. Moreover, the shape of the heater 1 is not limited to a columnar shape, and may have a desired shape such as a rod shape or a plate shape according to the application.
- the ceramic substrate 10 is an insulator.
- the heating resistor 20 is a conductor and is positioned inside the ceramic substrate 10 .
- the heating resistor 20 has terminals 20a and 20b at both ends.
- the heating resistor 20 generates heat by energization from lead wires (not shown) through terminals 20a and 20b.
- FIG. 2 is an enlarged view of area A shown in FIG. As shown in FIG. 2, the heater 1 is positioned such that the ceramic substrate 10 and the heating resistor 20 face each other with the interface 30 interposed therebetween.
- the ceramic base 10 has a plurality of crystal grains 17 and grain boundary phases 18 .
- Crystal grains 17 are made of silicon nitride. Crystal grains 17 may include Si 3 N 4 having ⁇ -phase crystals.
- the ceramic substrate 10 can have high strength and excellent heat resistance as compared with the case where the crystal grains 17 are made of other ceramic materials such as alumina or zirconia. , it is possible to use the heater 1 at higher temperatures.
- the ceramic substrate 10 may contain impurities such as SiAlON, SiC, Si 2 N 2 O, Mg silicon nitride compounds, in addition to the crystal grains 17 made of silicon nitride.
- the ceramic substrate 10 may also contain crystal grains 17 containing elements other than Si and N, such as O, C, and the like.
- the crystal grains 17 may have an aspect ratio of 1 or more and 2 or less.
- the aspect ratio is obtained by dividing the major axis by the minor axis of the crystal grains 17 of the ceramic substrate 10 .
- the major diameter is the length of the longest portion of the target crystal grain 17, and the minor diameter is the length of the longest portion in the direction perpendicular to the major diameter.
- the durability of the heater 1 can be further improved. That is, when the aspect ratio of the crystal grains 17 is 1 or more and 2 or less, heat conduction and heat-induced stress in the ceramic substrate 10 tend to be evenly transmitted in all directions. Therefore, part of the grain boundary phase 18 located between the plurality of crystal grains 17 present in the region 11 including the interface 30 with the heat generating resistor 20 is softened during energization, and the ceramic base 10 including the interface 30 is softened. The stress generated in the Therefore, the durability of the heater 1 can be further enhanced. That is, more crystal grains 17 having an aspect ratio of 1 or more and 2 or less may exist in the region 21 than in the region 22 .
- the grain boundary phase 18 is located between multiple crystal grains 17 .
- Grain boundary phase 18 is the first grain boundary phase containing oxides of rare earth elements and silicon.
- the grain boundary phase 18 refers to a portion of the grain boundaries that separate the adjacent crystal grains 17, where rare earth elements can be confirmed by Electron Probe Micro Analyzer (EPMA) analysis.
- the EPMA analysis can be performed by sampling the ceramic base portion of the heater 1, detecting the crystal grains 17 with a scanning electron microscope (SEM), and focusing on the crystal grains 17 for analysis.
- SEM scanning electron microscope
- rare earth elements can be identified by using wavelength dispersion spectroscopy.
- the grain boundary phase 18 contains oxides of rare earth elements and silicon.
- the grain boundary phase 18 contains a rare earth element and silicon oxide, for example, excessive softening of the ceramic base 10 due to heat generation of the heater 1 can be suppressed, and shape retention can be ensured.
- the grain boundary phase 18 may contain, for example, Yb, Y or Er as a rare earth element.
- the ceramic substrate 10 has regions 11 and 12 .
- Region 11 is an example of a first region
- region 12 is an example of a second region.
- the region 11 includes the interface 30 and refers to the portion facing the heating resistor 20 .
- the region 11 is, for example, a region with a thickness t11 from the interface 30 up to 0.5 mm.
- a region 12 is a portion farther from the heating resistor 20 than the region 11 .
- the region 12 is, for example, a region where the thickness t11 from the interface 30 exceeds 0.5 mm.
- thermal stress caused by repeated heating and cooling over a long period of time concentrates on the interface 30 between the ceramic substrate 10 and the heating resistor 20, and microcracks may occur at or near the interface 30. Continuing to use the heater 1 with microcracks may break the heating resistor 20 .
- the distribution amount of the grain boundary phase 18 differs between the regions 11 and 12 .
- the region 11 has a larger distribution amount of the grain boundary phase 18 than the region 12 .
- the distribution amount of the grain boundary phase 18 means the distribution area of the grain boundary phase 18 per unit area in each of the regions 11 and 12 of the ceramic substrate 10 viewed in cross section.
- the durability of the heater 1 can be improved. That is, in the heater 1 in which the distribution amount of the grain boundary phase 18 located in the region 11 including the interface 30 is larger than that in the region 12, the grain boundary located in the region 11 including the interface 30 with the heating resistor 20 is A portion of the phase 18 is softened and the stress generated in the ceramic substrate 10 including the interface 30 is relieved. For example, when microcracks occur in the vicinity of the boundary between the ceramic substrate 10 and the heating resistor 20 including the interface 30, part of the grain boundary phase 18 heated by energization of the heating resistor 20 is in the microcracks. It diffuses and fills microcracks. Thus, according to the heater 1 according to the embodiment, microcracks generated in the interface 30 can be self-repaired. Thereby, the durability of the heater 1 can be improved.
- region 12 has higher thermal conductivity than region 11 .
- the ceramic substrate 10 may have different average dimensions of the grain boundary phase 18 between the regions 11 and 12 .
- region 11 may have a larger average grain boundary phase 18 dimension than region 12 .
- the “average size of the grain boundary phase 18” means the average value of the size of each grain boundary phase 18 located per unit area in each of the regions 11 and 12 of the ceramic substrate 10 viewed in cross section. be.
- the "size of the grain boundary phase 18” is the equivalent circle diameter of each grain boundary phase 18 in each of the regions 11 and 12 of the ceramic base 10 as viewed in cross section.
- the durability of the heater 1 can be improved. That is, in the heater 1 in which the average size of the grain boundary phase 18 located in the region 11 including the interface 30 is larger than that of the region 12, the grain boundary located in the region 11 including the interface 30 with the heating resistor 20 is The absolute amount of softening components in the phase 18 increases. Therefore, the components of the softened grain boundary phase 18 reach, for example, microcracks generated near the interface 30, which is the boundary between the ceramic base 10 and the heating resistor 20, and are easily filled inside. Therefore, microcracks generated at the interface 30 can be self-repaired more accurately. Thereby, the durability of the heater 1 can be further improved.
- the ceramic substrate 10 may have different average sizes of the crystal grains 17 between the regions 11 and 12 .
- region 11 may have a larger average size of crystal grains 17 than region 12 .
- the "average size of the crystal grains 17" means the average value of the equivalent circle diameters of the crystal grains 17 located per unit area in the regions 11 and 12 of the ceramic substrate 10 viewed in cross section. be.
- the durability of the heater 1 can be improved. That is, when the average size of crystal grains 17 increases, the extension distance of cracks per crystal grain 17 tends to increase. Therefore, cracks generated in the crystal grains 17 located in the region 11 of the ceramic substrate 10 can reach the heating resistor 20 across the interface 30 and break the heating resistor 20, which can be reduced. Thereby, the durability of the heater 1 can be improved.
- the heating resistor 20 has a plurality of crystal grains 27 and a grain boundary phase 28.
- Crystal grains 27 include conductor grains 23 and insulator grains 26 .
- the conductor particles 23 consist of a conductor component.
- “composed of a conductor component” means that 99% by mass or more of the total components constituting the conductor particles 23 contain 99% by mass or more of the conductor component.
- the conductor particles 23 may contain tungsten or molybdenum as a conductor component.
- the conductor component contained in the conductor particles 23 may be tungsten carbide (WC).
- the conductor particles 23 may contain impurities of 1% by mass or less in addition to the conductor component.
- the insulator particles 26 are made of silicon nitride.
- “composed of silicon nitride” means that 99% by mass or more of silicon nitride is contained in 100% by mass of all the components constituting the insulator particles 26 .
- the insulator particles 26 may have acicular crystals 26a.
- the “needle-like crystal 26a” means a crystal structure elongated like a needle in one direction in the insulator particle 26 when viewed in cross section.
- the aspect ratio of the needle crystals 26a may be, for example, 3 or more and 20 or less.
- the insulator particles 26 may have a higher ratio of needle-like crystals than the crystal particles 17 of the ceramic substrate 10 .
- the ratio of the needle-like crystals 26a included in the insulator particles 26 larger than the ratio of the needle-like crystals included in the crystal grains 17, for example, the durability of the heater 1 can be enhanced.
- the durability of the heater 1 can be improved. That is, in the heating resistor 20, the needle-like crystals 26a are positioned so as to be entangled between the plurality of crystal grains 27, thereby improving the toughness of the region where the needle-like crystals 26a are positioned. Therefore, the heating resistor 20 having a smaller ratio of the needle crystals 26a to the insulating particles 26 has higher toughness than the ceramic substrate 10. Even if part of the grain boundary phase 28 located in the region 21 including the interface 30 is softened, the heat generating resistor 20 is less prone to microcracks. Therefore, durability of the heater 1 can be enhanced.
- the crystal grains 17 of the ceramic substrate 10 may not have needle-like crystals.
- the insulator particles 26 may include the first crystal 24 and the second crystal 25 .
- the first crystalline body 24 may be Si 3 N 4 having an ⁇ -phase crystal.
- the second crystalline body 25 may be Si 3 N 4 having a ⁇ -phase crystal.
- the heating resistor 20 may contain more first crystals 24 than second crystals 25 .
- the grain boundary phase 28 is located between multiple crystal grains 27 .
- Grain boundary phase 28 is an example of a second grain boundary phase containing oxides of rare earth elements and silicon.
- an element different from that of the crystal grains 27 is segregated by EPMA analysis among the grain boundaries partitioning the conductor grains 23 and/or the insulator grains 26 constituting the adjacent crystal grains 27. It means the part where you can confirm.
- the EPMA analysis can be performed by sampling the heating resistor 20 of the heater 1, detecting the crystal grains 27 with a scanning electron microscope (SEM), and focusing between the crystal grains 27 for analysis. Further, the element can be specified by using wavelength dispersion spectroscopy.
- the grain boundary phase 28 may be located between the conductor grains 23 and the insulator grains 26 that are adjacent to each other, or may be located between a plurality of conductor grains 23 or between a plurality of insulator grains 26 .
- the grain boundary phase 28 may contain oxides of rare earth elements and silicon, for example.
- the grain boundary phase 28 may contain, for example, Yb, Y or Er as a rare earth element.
- the primary sintered body or conductor paste which is the material of the heating resistor 20
- a rare earth element oxide for example, Yb 2 O 3
- the method of manufacturing the heater 1 is merely an example, and any method may be used.
- the heating resistor 20 may have regions 21 and 22 .
- Region 21 is an example of a third region
- region 22 is an example of a fourth region.
- the region 21 includes the interface 30 and refers to the portion facing the ceramic substrate 10 .
- the region 21 is, for example, a region with a thickness t21 from the interface 30 up to 0.2 mm.
- Region 22 refers to a portion farther from ceramic substrate 10 than region 21 .
- the region 22 is, for example, a region where the thickness t21 from the interface 30 exceeds 0.2 mm.
- the heating resistor 20 may have different distribution amounts of the grain boundary phase 28 between the regions 21 and 22 .
- the region 21 may have a larger distribution amount of the grain boundary phase 28 than the region 22 .
- the distribution amount of the grain boundary phase 28 means the distribution area of the grain boundary phase 28 per unit area in each of the regions 21 and 22 of the heating resistor 20 viewed in cross section.
- the durability of the heater 1 can be improved. That is, in the heater 1 in which the distribution amount of the grain boundary phase 28 located in the region 21 including the interface 30 is larger than that in the region 22, the grain boundary phase located in the region 21 including the interface 30 with the ceramic substrate 10 is A part of 28 is softened, and the stress generated in the heating resistor 20 including the interface 30 is relieved. For example, when microcracks occur in the vicinity of the boundary between the heating resistor 20 and the ceramic substrate 10 including the interface 30, part of the grain boundary phase 28 heated by the energization of the heating resistor 20 will be in the microcracks. It diffuses and fills microcracks. Thus, according to the heater 1 according to the embodiment, microcracks generated in the interface 30 can be self-repaired. Thereby, the durability of the heater 1 can be improved.
- the grain boundary phase 28 may have different average dimensions between the regions 21 and 22. Specifically, region 21 may have a larger average grain boundary phase 28 dimension than region 22 .
- the average size of the grain boundary phase 28 means the average value of the size of each grain boundary phase 28 located per unit area in each of the regions 21 and 22 of the heating resistor 20 viewed in cross section. is.
- the "size of the grain boundary phase 28” is the equivalent circle diameter of each grain boundary phase 28 in each of the regions 21 and 22 of the heating resistor 20 in cross section.
- the durability of the heater 1 can be improved. That is, in the heater 1 in which the average size of the grain boundary phase 28 located in the region 21 including the interface 30 is larger than that of the region 22, the grain boundary phase located in the region 21 including the interface 30 with the ceramic substrate 10 is 28, the absolute amount of softening components increases. Therefore, the components of the softened grain boundary phase 28 reach, for example, microcracks generated near the boundary between the heating resistor 20 including the interface 30 and the ceramic substrate 10, and are easily filled inside. Therefore, microcracks generated at the interface 30 can be self-repaired more accurately. Thereby, the durability of the heater 1 can be further improved.
- the heating resistor 20 may have different contents of the insulating particles 26 between the regions 21 and 22 .
- region 21 may have a higher content of insulator particles 26 than region 22 .
- the "content of insulator particles 26" means the total area of insulator particles 26 per unit area in each of regions 21 and 22 of heating resistor 20 when viewed in cross section.
- the durability of the heater 1 can be improved is, for example, the following. That is, the insulator grains 26 positioned in the region 21 are similar in composition to the crystal grains 17 positioned in the region 11 adjacent to the region 21 across the interface 30 . Therefore, by increasing the content of the insulating particles 26 located in the region 21 than in the region 22, the adhesion between the heat generating resistor 20 and the ceramic base 10 is enhanced, so that the durability of the heater 1 can be enhanced. can be done.
- the content of the insulator particles 26 is lower in the region 22 away from the interface 30 than in the region 21, the content of the conductor particles 23 is relatively higher in the region 22 than in the region 21. Since the area 22 of the heating resistor 20 has a larger amount of charge transfer per unit volume than the area 21, the durability of the heater 1 is improved even when the heater 1 is used at a high output. can be enhanced.
- the heating resistor 20 may have different average dimensions of the insulator particles 26 between the regions 21 and 22 .
- region 21 may have a larger average size of insulator grains 26 than region 22 .
- the “average size of the insulator particles 26” refers to the average value of the circle-equivalent diameters of the insulator particles 26 located per unit area in the regions 21 and 22 of the heating resistor 20 when viewed in cross section. It's about.
- insulator particles 26 with a larger average size tend to be more impact resistant than insulator particles 26 with a smaller average size.
- the strength of the region 21 including the interface 30 where stress tends to concentrate can keep Therefore, durability of the heater 1 can be enhanced.
- the insulator particles 26 adjacent to the conductor particles 23 with a smaller average size are more likely to release stress. easier.
- the amount of charge movement per unit time is larger than in the region 21. Therefore, the average size of the insulator particles 26 located in the region 22 is equal to that of the insulator particles 26 located in the region 21.
- the average size of crystal grains made of silicon nitride may differ between the regions 11 and 21 adjacent to each other with the interface 30 interposed therebetween.
- the crystalline grains 17 located in region 21 may have a larger average size than the insulator grains 26 located in region 22 .
- the region 11 having the crystal grains 17 having a large average size has an improved thermal conductivity compared to the region 22 having the insulating grains 26 having a small average size. Therefore, the thermal stress generated in the region 11 near the heating resistor 20 can be relieved, so that the durability of the heater 1 can be enhanced.
- the crystal grains 17 and the grain boundary phase 18 of the ceramic substrate 10, and the crystal grains 27 (the conductor particles 23 and the insulator grains 26) and the grain boundary phase 28 of the heating resistor 20 were obtained by observing the cross section of the heater 1 by EPMA analysis. , it is possible to confirm its location. Also, the size and average size of the crystal grains 17 and the grain boundary phase 18 can be calculated based on the result of observing the cross section of the ceramic substrate 10 with an SEM. Also, the crystal structures of the crystal grains 17 and the insulator grains 26 can be measured using an X-ray diffractometer (XRD).
- XRD X-ray diffractometer
- the heater 1 includes the ceramic substrate 10 and the heating resistor 20.
- the ceramic substrate 10 has a plurality of crystal grains 17 made of silicon nitride and a first grain boundary phase (grain boundary phase 18) located between the plurality of crystal grains 17 and containing an oxide of a rare earth element and silicon. .
- the heating resistor 20 is positioned inside the ceramic base 10 .
- the ceramic substrate 10 has a first region (region 11) including an interface 30 with the heating resistor 20 and a second region (region 12) farther from the heating resistor 20 than the first region.
- the first region has a larger distribution amount of the first grain boundary phase than the second region. This makes it possible to provide the heater 1 with high durability.
- the average size of the first grain boundary phase is larger than that in the second region. This makes it possible to provide the heater 1 with high durability.
- the heating resistor 20 includes a plurality of crystal grains 27 made of a conductor component or silicon nitride, and second grain boundaries located between the plurality of crystal grains 27 and containing a rare earth element and silicon oxide.
- the average size of the second grain boundary phase is larger than that in the fourth region. This makes it possible to provide the heater 1 with high durability.
- the third region according to the embodiment contains more crystal grains made of silicon nitride than the fourth region. This makes it possible to provide the heater 1 with high durability.
- the crystal grains made of silicon nitride contained in the heating resistor 20 according to the embodiment have a larger ratio of the needle crystals 26 a than the crystal grains 17 made of silicon nitride contained in the ceramic substrate 10 . This makes it possible to provide the heater 1 with high durability.
- the aspect ratio of the crystal grains 17 made of silicon nitride contained in the ceramic substrate 10 according to the embodiment is 1 or more and 2 or less. This makes it possible to provide the heater 1 with high durability.
- REFERENCE SIGNS LIST 1 heater 10 ceramic substrate 17, 27 crystal grains 18, 28 grain boundary phase 20 heating resistor 23 conductive particles 24 first crystal 25 second crystal 26 insulator particles 30 interface
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- Ceramic Engineering (AREA)
- Resistance Heating (AREA)
Abstract
Description
10 セラミック基体
17,27 結晶粒子
18,28 粒界相
20 発熱抵抗体
23 導体粒子
24 第1結晶体
25 第2結晶体
26 絶縁体粒子
30 界面
Claims (7)
- 窒化珪素からなる複数の結晶粒子と、該複数の結晶粒子間に位置し、希土類元素および珪素の酸化物を含む第1粒界相とを有するセラミック基体と、
前記セラミック基体の内部に位置する発熱抵抗体と
を備え、
前記セラミック基体は、前記発熱抵抗体との界面を含む第1領域と、前記第1領域よりも前記発熱抵抗体から離れた第2領域とを有し、
前記第1領域は、前記第2領域よりも前記第1粒界相の分布量が多い
ヒータ。 - 前記第1領域は、前記第2領域よりも前記第1粒界相の平均寸法が大きい
請求項1に記載のヒータ。 - 前記発熱抵抗体は、導体成分または窒化珪素からなる複数の結晶粒子と、該複数の結晶粒子間に位置し、希土類元素および珪素の酸化物を含む第2粒界相とを有するとともに、前記セラミック基体との界面を含む第3領域と、前記第3領域よりも前記セラミック基体から離れた第4領域とを有し、
前記第3領域は、前記第4領域よりも前記第2粒界相の分布量が多い
請求項1または2に記載のヒータ。 - 前記第3領域は、前記第4領域よりも前記第2粒界相の平均寸法が大きい
請求項3に記載のヒータ。 - 前記第3領域は、前記第4領域よりも前記窒化珪素からなる複数の結晶粒子の含有量が多い
請求項3または4に記載のヒータ。 - 前記発熱抵抗体に含まれる窒化珪素からなる結晶粒子は、前記セラミック基体に含まれる前記窒化珪素からなる結晶粒子よりも針状結晶の割合が大きい
請求項1~5のいずれか1つに記載のヒータ。 - 前記セラミック基体に含まれる前記窒化珪素からなる結晶粒子のアスペクト比は、1以上2以下である
請求項1~6のいずれか1つに記載のヒータ。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202280013600.4A CN116848945A (zh) | 2021-03-04 | 2022-03-03 | 加热器 |
US18/276,270 US20240114596A1 (en) | 2021-03-04 | 2022-03-03 | Heater |
JP2023503951A JPWO2022186344A1 (ja) | 2021-03-04 | 2022-03-03 |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH09245940A (ja) * | 1996-03-06 | 1997-09-19 | Jidosha Kiki Co Ltd | セラミック発熱体およびその製造方法 |
JP2001267044A (ja) * | 2000-03-23 | 2001-09-28 | Ngk Spark Plug Co Ltd | セラミックヒータ及びその製造方法 |
JP2014157010A (ja) * | 2013-01-21 | 2014-08-28 | Ngk Spark Plug Co Ltd | グロープラグ |
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- 2022-03-03 CN CN202280013600.4A patent/CN116848945A/zh active Pending
- 2022-03-03 WO PCT/JP2022/009188 patent/WO2022186344A1/ja active Application Filing
- 2022-03-03 US US18/276,270 patent/US20240114596A1/en active Pending
- 2022-03-03 JP JP2023503951A patent/JPWO2022186344A1/ja active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09245940A (ja) * | 1996-03-06 | 1997-09-19 | Jidosha Kiki Co Ltd | セラミック発熱体およびその製造方法 |
JP2001267044A (ja) * | 2000-03-23 | 2001-09-28 | Ngk Spark Plug Co Ltd | セラミックヒータ及びその製造方法 |
JP2014157010A (ja) * | 2013-01-21 | 2014-08-28 | Ngk Spark Plug Co Ltd | グロープラグ |
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JPWO2022186344A1 (ja) | 2022-09-09 |
CN116848945A (zh) | 2023-10-03 |
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