WO2021235407A1 - Procédé de production de plaque en céramique, procédé de production de support d'enfournement et procédé de régénération de support d'enfournement - Google Patents

Procédé de production de plaque en céramique, procédé de production de support d'enfournement et procédé de régénération de support d'enfournement Download PDF

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WO2021235407A1
WO2021235407A1 PCT/JP2021/018676 JP2021018676W WO2021235407A1 WO 2021235407 A1 WO2021235407 A1 WO 2021235407A1 JP 2021018676 W JP2021018676 W JP 2021018676W WO 2021235407 A1 WO2021235407 A1 WO 2021235407A1
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Prior art keywords
setter
ceramic green
green sheet
contact surface
ceramic
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PCT/JP2021/018676
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English (en)
Japanese (ja)
Inventor
利貴 山縣
満博 山口
里樹 東
江 尹
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デンカ株式会社
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Priority to JP2022524473A priority Critical patent/JP7185099B2/ja
Publication of WO2021235407A1 publication Critical patent/WO2021235407A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—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
    • C04B35/584—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 silicon nitride
    • C04B35/587—Fine ceramics
    • 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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes

Definitions

  • This disclosure relates to a method for manufacturing a ceramic plate, a method for manufacturing a setter, and a method for regenerating a setter.
  • Power modules that control large currents are used in fields such as automobiles, electric railways, industrial equipment, and power generation.
  • the circuit board mounted on the power module has an insulating ceramic plate.
  • a method for manufacturing a ceramic plate for example, the following manufacturing method as described in Patent Document 1 is known. That is, a step of extruding the ceramic powder into a sheet after mixing it with a sintering aid or the like, a step of punching to form a ceramic green sheet, and a step of firing the ceramic green sheet are performed. Then, a ceramic plate is manufactured. In the firing step of the ceramic green sheet, the ceramic green sheet is fired in a state where about 10 to 20 ceramic green sheets are laminated on the setter.
  • the present disclosure provides a method for manufacturing a ceramic plate, which can improve the production efficiency of the ceramic plate by regenerating the setter. Further, the present invention provides a method for manufacturing a setter and a method for regenerating the setter, which can effectively utilize resources.
  • the method for manufacturing a ceramic plate includes a first firing step of laminating and firing the setter and the first ceramic green sheet so as to be in contact with each other to obtain a ceramic plate, and a first ceramic green sheet.
  • the heating step of heating the setter with at least a part of the contact surface of the setter exposed and the second ceramic green sheet are laminated and fired so as to be in contact with each other at at least a part of the contact surface. It has a second firing step of obtaining a ceramic plate.
  • the setter is heated with at least a part of the contact surface of the setter exposed, which was in contact with the first ceramic green sheet.
  • the temperature may be higher than the temperature at which the foreign matter containing a component different from the component contained in the setter that adheres to the contact surface is decomposed.
  • the "component contained in the setter” in the present disclosure refers to a component originally contained in the setter before it is used in the method for manufacturing a ceramic plate. That is, it is a component (constituent component) contained in an unused setter.
  • the component contained in the setter composed of the boron nitride sintered body is boron nitride.
  • a plurality of setters including the above setter and a plurality of first ceramic green sheets including the first ceramic green sheet may be laminated and fired so as to be in contact with each other.
  • the plurality of setters may be heated with the contact surfaces of the plurality of setters in contact with the first ceramic green sheet separated from each other. This allows a plurality of setters to be heated and regenerated together. Therefore, the production efficiency of the ceramic plate can be further improved.
  • the first ceramic green sheet contains silicon nitride
  • the setter may be heated at 1450 to 2000 ° C. in an atmosphere of an inert gas.
  • the decomposition of silicon nitride contained in the foreign matter proceeds smoothly, and the time required for the heating step can be shortened.
  • foreign matter on the contact surface of the setter can be sufficiently reduced, and unevenness generated on the surface of the ceramic plate obtained in the second firing step can be further reduced.
  • the method for manufacturing a setter according to one aspect of the present disclosure is different from the components contained in the first setter on the contact surface with the ceramic green sheet by laminating and firing so that the first setter and the ceramic green sheet are in contact with each other. It has a firing step of obtaining a second setter to which foreign matter containing a component is attached, and a heating step of heating the second setter with at least a part of the contact surface exposed to reduce foreign matter on the contact surface. ..
  • the above-mentioned manufacturing method has a heating step of heating the second setter in which foreign matter adheres to the contact surface with the ceramic green sheet in the firing step.
  • the second setter is heated with at least a part of the contact surface exposed to reduce foreign matter on the contact surface.
  • the setter (third setter) obtained by reducing the amount of foreign matter can be laminated and fired so as to be in contact with the ceramic green sheet again.
  • the waste amount of the setter can be reduced and the resources can be effectively utilized by manufacturing the setter (third setter) in which the foreign matter is reduced from the second setter to which the foreign matter is attached. can.
  • the temperature may be higher than the temperature at which the foreign matter decomposes. As a result, foreign matter adhering to the contact surface can be sufficiently and smoothly reduced. Therefore, the setter can be efficiently manufactured.
  • a plurality of first setters including the first setter and a plurality of ceramic green sheets including the ceramic green sheet are laminated and fired so as to be in contact with each other, and a plurality of second setsters including the second setter are fired. You may get 2 setters.
  • the plurality of second setters may be heated with the contact surfaces of the plurality of second setters in contact with the ceramic green sheet separated from each other. Thereby, a plurality of second setters can be heated together to produce a plurality of setters at the same time. Therefore, the production efficiency of the setter can be improved.
  • the ceramic green sheet contains silicon nitride, and in the heating step, the second setter may be heated at 1450 to 2000 ° C. in an atmosphere of an inert gas.
  • the decomposition of silicon nitride contained in the foreign matter proceeds smoothly, and the time required for the heating step can be shortened.
  • the method for regenerating a setter according to one aspect of the present disclosure is different from the components contained in the first setter on the contact surface with the ceramic green sheet by laminating and firing so that the first setter and the ceramic green sheet are in contact with each other. It has a firing step of obtaining a second setter to which foreign matter containing a component is attached, and a heating step of heating the second setter with at least a part of the contact surface exposed to reduce foreign matter on the contact surface.
  • the above-mentioned regeneration method has a heating step of heating the second setter in which foreign matter adheres to the contact surface with the ceramic green sheet in the firing step.
  • the second setter is heated with at least a part of the contact surface exposed to reduce foreign matter on the contact surface.
  • the setter (third setter) obtained by reducing the amount of foreign matter can be laminated and fired so as to be in contact with the ceramic green sheet again.
  • the waste amount of the setter can be reduced and the resources can be effectively utilized by regenerating the setter (third setter) in which the foreign matter is reduced from the second setter to which the foreign matter is attached. can.
  • the present disclosure it is possible to provide a method for manufacturing a ceramic plate capable of improving the production efficiency of the ceramic plate by regenerating the setter. Further, it is possible to provide a method for manufacturing a setter and a method for regenerating the setter that can effectively utilize resources.
  • FIG. 6 is an SEM photograph showing an example of foreign matter (boron nitride particles) adhering to the contact surface of a setter made of a boron nitride sintered body. It is a figure which shows an example of a heating process. It is an SEM photograph which shows the main surface (before firing) of the setter used in Example 1.
  • FIG. 6 is an SEM photograph showing the main surface of FIG. 4 taken at a higher magnification than that of FIG.
  • FIG. 6 is an SEM photograph which shows the contact surface of the setter after the 1st firing step of Example 1.
  • FIG. 6 is an SEM photograph showing the contact surface of FIG. 6 taken at a higher magnification than that of FIG.
  • FIG. 6 is an SEM photograph showing the contact surface of FIG. 8 taken at a higher magnification than that of FIG. 6 is an SEM photograph showing the contact surface of the setter after the heating step of Comparative Example 1.
  • 11 is an SEM photograph showing the contact surface of FIG. 10 taken at a higher magnification than that of FIG. 11. It is a photograph which shows the example of the convex part on the surface of a silicon nitride plate.
  • a laminated body (first laminated body) laminated so that a setter and a ceramic green sheet (first ceramic green sheet) are in contact with each other is fired to obtain a ceramic plate.
  • the second firing to obtain a ceramic plate by firing the laminated body (second laminated body) in which the setter and the ceramic green sheet (second ceramic green sheet) are laminated so as to be in contact with each other at at least a part of the contact surface. It has a process.
  • the first ceramic green sheet and the second ceramic green sheet are ceramic green sheets laminated so as to be in contact with the setter.
  • the first ceramic green sheet and the second ceramic green sheet laminated so as to be in contact with the setter in the first firing step and the second firing step are manufactured by, for example, the following procedure.
  • First, a raw material slurry containing a ceramic powder, a sintering aid and a binder is formed.
  • the ceramic is not particularly limited, and examples thereof include carbides, oxides, and nitrides. Specific examples thereof include silicon carbide, alumina, silicon nitride, aluminum nitride and boron nitride.
  • Binders include those containing organic components.
  • first ceramic green sheet and a second ceramic green sheet may be processed into a desired shape by, for example, cutting.
  • the materials and shapes of the first ceramic green sheet and the second ceramic green sheet may be the same or different.
  • the setter for example, a commercially available ceramic sintered body may be purchased, or may be manufactured by a known method.
  • the setter include those containing at least one selected from the group consisting of boron nitride, silicon carbide, alumina, zirconia, graphite, and silicon nitride.
  • a setter made of boron nitride is preferably used because it has both heat resistance and good machinability.
  • the material of the setter may be different from the material of the ceramic plate from the viewpoint of suppressing the adhesion between the setter and the ceramic plate after firing.
  • a boron nitride sintered body When a boron nitride sintered body is used as the setter, it can be manufactured by the following procedure. First, a molded product is produced using hexagonal boron nitride powder as a raw material. If necessary, a sintering aid may be added to the hexagonal boron nitride powder before molding. Examples of the sintering aid include alkaline earth oxides such as magnesium oxide and calcium oxide, rare earth oxides such as aluminum oxide, silicon oxide and yttrium oxide, and composite oxides such as spinel.
  • the molding may be performed by uniaxial pressure molding and CIP molding. Uniaxial pressure molding may be performed at 3 to 20 MPa. CIP molding may be performed at 50 to 300 MPa.
  • the obtained molded product is fired to obtain a boron nitride sintered body.
  • the firing may be carried out under the conditions of a non-oxidizing atmosphere, a heating rate of 150 ° C./hr or less, a maximum temperature of 1800 to 2200 ° C., and a holding time of 5 hours or more in this temperature range.
  • the non-oxidizing atmosphere include a nitride gas atmosphere such as nitrogen and ammonia.
  • the density of the boron nitride sintered body may be 1600 kg / m 3 or more.
  • the method for producing the boron nitride sintered body is not limited to the above method. For example, it may be manufactured by a hot press method. Ceramic sintered bodies other than the boron nitride sintered body can be produced by a known method.
  • the setter thus obtained and the first ceramic green sheet are laminated so as to be in contact with each other to produce a laminated body.
  • the number of setters and ceramic green sheets constituting the laminate is not particularly limited.
  • As the laminate for example, a plurality of (for example, 50 to 100) ceramic green sheets including the first ceramic green sheet may be sandwiched between a pair of setters. Further, one setter and a plurality of ceramic green sheets including the first ceramic green sheet may be arranged alternately. As described above, by firing a plurality of ceramic green sheets in the first firing step, a plurality of ceramic plates can be manufactured at the same time.
  • the material and shape of the ceramic green sheet laminated together with the first ceramic green sheet may be the same as or different from that of the first ceramic green sheet.
  • a mold release agent may be applied to the main surface of the ceramic green sheet (first ceramic green sheet) in order to prevent the adjacent ceramic green sheets from adhering to each other during firing. Further, the mold release agent may be applied to the surface of the setter facing the main surface of the first ceramic green sheet. Examples of the component contained in the release agent include ceramic powder such as boron nitride, graphite powder, and binder.
  • FIG. 1 is a diagram illustrating an example of the first firing step of the laminated body.
  • the laminate 50 includes three setters 10 and a plurality of ceramic green sheets 30.
  • the plurality of ceramic green sheets 30 include four first ceramic green sheets 30a adjacent to the three setters 10.
  • the pair of setters 10A and 10B are laminated at the bottom and top of the laminated body 50. Therefore, in the setters 10A and 10B, one main surface is in contact with the first ceramic green sheet 30a.
  • the remaining setter 10C is laminated in the central portion of the laminated body 50. Therefore, both main surfaces of the setter 10C are in contact with the first ceramic green sheet 30a.
  • the contact surface of the setter 10 in which the first ceramic green sheet 30a and the setter 10 come into contact with each other is included in one or both main surfaces.
  • the laminated body 50 is housed in a degreasing furnace 20 and heated to, for example, 300 ° C. to 700 ° C. As a result, the binder contained in the ceramic green sheet 30 is removed. Subsequently, the degreased laminate 50 is housed in the firing furnace 25 and heated to 1600 ° C to 2000 ° C. As a result, the ceramic green sheet is fired and a ceramic plate is obtained.
  • the degreasing furnace 20 used for degreasing and the firing furnace 25 used for firing may be the same furnace or different furnaces. Further, the heating temperature, time and atmosphere may be appropriately adjusted according to the composition of the ceramic green sheet.
  • the laminated body (first laminated body) fired in the first firing step is separated into a ceramic plate and a setter.
  • the obtained ceramic plate may be processed as necessary to form, for example, a circuit board.
  • Granular foreign matter containing a component different from the component contained in the setter adheres to the contact surface that has been in contact with the first ceramic green sheet 30a (ceramic plate) of the separated setter.
  • the components contained in the foreign substance include components contained in a ceramic green sheet or a ceramic plate, and reaction products of these components and components contained in a setter.
  • the particle size of the foreign matter may be larger than the particles constituting the setter. That is, the foreign matter may be coarse particles.
  • FIG. 2 is an SEM photograph showing an example of foreign matter (boron nitride particles) adhering to the contact surface of a setter composed of a boron nitride sintered body.
  • the composition of foreign matter can be measured by EDS analysis.
  • the setter is composed of a boron nitride sintered body and the foreign matter is silicon nitride particles, it is difficult to find the foreign matter with the naked eye because the colors of both are similar.
  • the presence or absence of a foreign substance can be determined by performing SEM observation at a high magnification (for example, 500 times or more) as shown in FIG.
  • the setter with such foreign matter adhering to the contact surface is heated with the contact surface exposed.
  • foreign matter adhering to the contact surface can be volatilized or decomposed and reduced.
  • the heating may be carried out in an atmosphere of an inert gas.
  • the inert gas include nitrogen gas and argon gas.
  • the heating temperature in the heating step may be higher than the firing temperature in the first firing step, and may be higher than the temperature at which the foreign matter is decomposed.
  • the specific heating temperature may be, for example, 1450 ° C. or higher, 1600 ° C. or higher, or 1700 ° C. or higher.
  • the heating temperature may be, for example, 2000 ° C. or lower, 1950 ° C. or lower, or 1900 ° C. or lower.
  • the heating time at the above heating temperature may be, for example, 0.5 to 10 hours, or may be 1 to 5 hours.
  • FIG. 3 is a diagram illustrating an example of a heating process.
  • a plurality of setters 11 are stacked on the bottom plate 13.
  • Spacers 12 are arranged between the setters 11 adjacent to each other in the vertical direction.
  • the contact surfaces of the adjacent setters 11 are arranged so as to be separated from each other at a predetermined interval.
  • a part or all of the contact surface included in the main surface of the setter 11 is heated in the heating furnace 28 in an exposed state.
  • the same one as that of the firing furnace 25 of FIG. 1 may be used, or a different one may be used.
  • the plurality of setters 11 can be regenerated at the same time.
  • each setter 11 may be heated one by one. Further, it is not essential to use the spacer 12, and it suffices if the contact surface of each setter 11 can be heated in an exposed state. For example, using a frame having a support portion that supports the setter 11, a plurality of setters may be heated in a state of being arranged horizontally or vertically so that the contact surfaces are separated from each other.
  • the setter and the second ceramic green sheet are laminated so that the second ceramic green sheet comes into contact with at least a part of the contact surface of the setter whose foreign matter has been reduced in the heating step (second).
  • 2 laminated body is produced.
  • This second laminated body is heated in a degreasing furnace and a firing furnace to obtain a ceramic plate.
  • the degreasing furnace and the firing furnace may be the same as those used in the first firing step, or may be different.
  • the second laminated body may have the same laminated structure as the first laminated body 50 produced in the first firing step, or may have a different laminated structure.
  • the ceramic plate can be obtained by sequentially performing degreasing and firing in the same manner as in the first firing step.
  • the setter comes into contact with the second ceramic green sheet on the contact surface where foreign matter is reduced. Therefore, foreign matter on the contact surface between the second ceramic green sheet and the setter is reduced. Therefore, it is possible to prevent the ceramic plate obtained in the second firing step from having irregularities. In this way, the yield of the ceramic plate can be maintained even if the setter used in the first firing step is reused. Therefore, the production efficiency of the ceramic plate can be improved.
  • the heating step and the second firing step may be repeated.
  • the number of repetitions may be once or multiple times.
  • the setter may be heated with the contact surface with the second ceramic green sheet exposed each time the laminate is fired, or the laminate may be manufactured, the laminate may be fired, and the ceramic plate and the setter may be heated.
  • the heating step may be performed after the sorting is repeated a plurality of times.
  • the frequency of the heating step may be adjusted according to the presence or absence of foreign matter on the contact surface or the amount of foreign matter. In any case, by repeatedly regenerating and using the setter, it is possible to effectively utilize resources and reduce the manufacturing cost of the ceramic plate.
  • the ceramic plates obtained in the first firing step and the second firing step of the above-mentioned manufacturing method have the same surface quality. Therefore, it can be used for the same purpose.
  • the ceramic plate may be used as a circuit board by forming an electric circuit composed of a metal layer on one or both main surfaces, for example.
  • a laminated body in which the first setter and the ceramic green sheet are laminated so as to be in contact with each other is fired, and the contact surface of the first setter is formed on the contact surface with the ceramic green sheet.
  • the firing step can be performed in the same manner as the first firing step described above. That is, the first setter may be a commercially available ceramic sintered body or may be manufactured by a known method. Examples of the setter include those composed of at least one selected from the group consisting of boron nitride, silicon carbide, alumina, zirconia, graphite, and silicon nitride. The manufacturing procedure when the boron nitride sintered body is used as the first setter may be as described above. In the firing step, the laminate as shown in FIG. 1 may be housed in the firing furnace 25 and heated.
  • first setter the setter before firing in the firing step (first firing step)
  • second setter the setter baked in the firing step and having foreign matter adhered to the contact surface
  • the laminate obtained in the firing step is separated into a ceramic plate and a second setter, and the second setter is in a state where at least a part of the contact surface with the ceramic green sheet (ceramic plate) of the second setter is exposed. Heat the setter. As a result, the foreign matter adhering to the contact surface is volatilized or decomposed, and the foreign matter can be reduced.
  • a setter in which foreign matter is reduced by the heating step in this way may be referred to as a "third setter".
  • the heating conditions in the heating step may be the same as the heating step in the embodiment of the method for manufacturing a ceramic plate described above. Foreign matter adhering to the surface of the setter (third setter) obtained by the heating step is sufficiently reduced.
  • This setter (third setter) may have, for example, the same surface quality as the first setter.
  • the setter (third setter) thus obtained through the heating step may be used in the firing step (second firing step) instead of the first setter.
  • the second setter in which the foreign matter adheres to the contact surface is obtained again together with the ceramic plate. After this, the heating step may be performed again.
  • the used second setter can be regenerated as the third setter, and the amount of waste of the second setter can be reduced.
  • the second firing step and the heating step may be repeated a plurality of times. In this case, the reproduction of the second setter to the third setter and the production of the ceramic plate using the third setter (generation of the second setter) are repeatedly performed. Therefore, effective use of resources can be further promoted.
  • the setter manufacturing method of the present embodiment heats the used second setter used in the firing step to newly create a setter (third setter) in which foreign matter on the surface is reduced. Corresponds to the manufacturing method of. From another point of view, since the used setter is surface-treated and the used setter is regenerated, it can be said that the setter is surface-treated or the setter is regenerated.
  • the ceramic plate, the ceramic green sheet, and the setter may have a shape other than the rectangular parallelepiped shape. These may be chamfered at the corners. Further, the setter may be arranged only below the laminated body.
  • Example 1 Manufacturing of ceramic plates and regeneration of setters.
  • Example 1 A molded body (sheet material) was prepared by uniaxial pressure molding of a raw material powder containing silicon nitride powder and a sintering aid (magnesium oxide powder, yttrium oxide powder and silicon dioxide powder). This sheet material was punched out using a cutting device to form 68 ceramic green sheets having a rectangular parallelepiped shape.
  • three setters made of boron nitride having a rectangular parallelepiped shape manufactured by Denka Co., Ltd., trade name: NB-1000
  • FIG. 4 is an SEM photograph (100 times) of the main surface (before firing) of the setter.
  • FIG. 4 is an SEM photograph (100 times) of the main surface (before firing) of the setter.
  • FIG. 5 is an SEM photograph (500 times) of the main surface (before firing) of the setter taken at a higher magnification than that of FIG. As shown in FIGS. 4 and 5, no foreign matter was detected on the main surface of the setter (first setter) before firing. In the following, a laminate was produced so that the main surface and the ceramic green sheet were in contact with each other.
  • 34 ceramic green sheets were stacked between the lower setter and the central setter, and between the central setter and the upper setter.
  • a slurry for mold release was applied to the contact surface of the setter with the ceramic green sheet and one main surface of each ceramic green sheet.
  • the degreasing furnace and a firing furnace the prepared laminate was degreased and fired.
  • the degreasing temperature was 500 ° C. and the degreasing time was 30 hours.
  • the firing temperature was 1800 ° C. and the firing time was 30 hours.
  • the laminate was taken out from the firing furnace, the ceramic plate was removed from the laminate, and a pair of setters were recovered.
  • FIG. 6 is an SEM photograph (100 times) of the contact surface of the setter recovered from the laminated body.
  • FIG. 7 is an SEM photograph (500 times) of the contact surface of the setter taken at a higher magnification than that of FIG. Although the presence of foreign matter could not be confirmed visually, when the contact surface was observed at a high magnification (about 500 times) using an SEM as shown in FIG. 7, it was confirmed that the foreign matter 40 had adhered. When EDS analysis of this foreign substance was performed, Si and N were detected. From this, it was confirmed that the silicon nitride particles, which are the components contained in the ceramic green sheet (ceramic plate), were present as foreign substances on the contact surface of the setter.
  • ⁇ Heating process> As shown in FIG. 3, three setters (three second setters) confirmed to have foreign matter attached to the contact surface were stacked via spacers and placed in the firing furnace. The portion of the contact surface to which foreign matter adhered was exposed to the space inside the firing furnace without contacting the spacer. Using a calcining furnace, three setters were heated at 1850 ° C. for 2 hours in a nitrogen gas atmosphere.
  • FIG. 8 is an SEM photograph (100 times) of the contact surface of the setter after heating in the heating step.
  • FIG. 9 is an SEM photograph (500 times) of the contact surface of the setter taken at a higher magnification than that of FIG.
  • FIG. 9 shows the contact surface of the setter magnified at the same magnification as in FIG. As shown in FIG. 9, the heating process sufficiently reduced the foreign matter adhering to the contact surface.
  • Example 1 The firing step was carried out in the same manner as in Example 1 to obtain three setters (three second setters) to which foreign matter adhered to the contact surface.
  • the heating step was performed in the same manner as in Example 1 except that the contact surfaces of the three setters were stacked so as to be in contact with each other and heated in the firing furnace. That is, the three setters were fired so that the contact surfaces of the three setters were not exposed to the space inside the firing furnace.
  • FIG. 10 is an SEM photograph (100 times) of the contact surface of the setter after heating in the heating step.
  • FIG. 11 is an SEM photograph (500 times) of the contact surface of the setter taken at a higher magnification than that of FIG. As shown in FIGS. 10 and 11, foreign matter 42 that had grown and coarsened in the heating step was present on the contact surface of the setter.
  • FIG. 12 is a photograph showing an example of a convex portion on the surface of the silicon nitride plate obtained in the second firing step. In FIG. 12, a convex portion 60 formed in the central portion of the main surface of the silicon nitride plate is shown.
  • each silicon nitride plate obtained in the second firing step of Example 1 and Comparative Example 1 was evaluated. Specifically, the main surface of the silicon nitride plate was observed with a one-shot 3D shape measuring machine (model: VR-3000) manufactured by KEYENCE CORPORATION, and the size of the unevenness on the surface was examined. A defective product was determined to have a convex portion having a height of 11 ⁇ m or more or a concave portion having a depth of 11 ⁇ m or more. As a result, in Example 1, the ratio of defective products could be reduced to 1/3 or less as compared with Comparative Example 1.

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Abstract

Procédé de production de plaque en céramique comprenant une première étape de cuisson dans laquelle un support d'enfournement et une première feuille crue en céramique sont stratifiés en contact l'un avec l'autre et sont cuits pour obtenir une plaque en céramique, une étape de chauffage dans laquelle le support d'enfournement est chauffé dans un état dans lequel au moins une partie de la surface de contact du support d'enfournement avec la première feuille en céramique crue est exposée, et une seconde étape de cuisson dans laquelle le support d'enfournement et une seconde feuille crue en céramique sont stratifiés en contact l'un avec l'autre dans au moins une partie de la surface de contact susmentionnée, et sont cuits pour obtenir une plaque en céramique.
PCT/JP2021/018676 2020-05-19 2021-05-17 Procédé de production de plaque en céramique, procédé de production de support d'enfournement et procédé de régénération de support d'enfournement WO2021235407A1 (fr)

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JP2008254962A (ja) * 2007-04-04 2008-10-23 Inax Corp セッターの平坦化処理方法
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Publication number Priority date Publication date Assignee Title
WO2023038151A1 (fr) * 2021-09-13 2023-03-16 デンカ株式会社 Procédé de production d'un corps fritté de nitrure de bore et corps fritté de nitrure de bore
JP7282279B1 (ja) * 2021-09-13 2023-05-26 デンカ株式会社 窒化ホウ素焼結体の製造方法及び窒化ホウ素焼結体

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