JP6876635B2 - Baking setter - Google Patents

Baking setter Download PDF

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JP6876635B2
JP6876635B2 JP2018002151A JP2018002151A JP6876635B2 JP 6876635 B2 JP6876635 B2 JP 6876635B2 JP 2018002151 A JP2018002151 A JP 2018002151A JP 2018002151 A JP2018002151 A JP 2018002151A JP 6876635 B2 JP6876635 B2 JP 6876635B2
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layer
base material
intermediate layer
coating layer
coating
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JP2019119659A (en
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常夫 古宮山
常夫 古宮山
貴博 水野
貴博 水野
浩臣 松葉
浩臣 松葉
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NGK Insulators Ltd
NGK Adrec Co Ltd
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NGK Insulators Ltd
NGK Adrec Co Ltd
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Priority to JP2018002151A priority Critical patent/JP6876635B2/en
Priority to CN201811388853.1A priority patent/CN110015903A/en
Priority to KR1020190001091A priority patent/KR102525393B1/en
Priority to TW108100502A priority patent/TWI811283B/en
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens, or the like for the charge within the furnace
    • F27D5/0006—Composite supporting structures
    • F27D5/0012—Modules of the sagger or setter type; Supports built up from them
    • 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
    • C04B35/56—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 carbides or oxycarbides
    • C04B35/565—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 carbides or oxycarbides based on silicon carbide
    • 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
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
    • 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
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D5/00—Supports, screens, or the like for the charge within the furnace
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/401—Alkaline earth metals
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/405—Iron group metals
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/422—Carbon
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
    • C04B2235/428—Silicon

Description

本明細書は、焼成用セッターに関する技術を開示する。 This specification discloses a technique relating to a firing setter.

被焼成物を焼成する際、被焼成物を載置するためにセッター等の焼成用治具が用いられる。特許文献１の焼成用セッター（焼成用容器）は、基材と被焼成物が反応することを抑制するため、基材表面にアルミニウム質、ジルコニア質のコーティング層を形成している。特許文献１では、コーティング材の粒径を調整し、その結果コーティング層の気孔率が調整され、基材とコーティング層の熱膨張差に起因する両者の剥離を抑制している。しかしながら、コーティング層と基材の剥離を抑制するためにコーティング材の粒径を調整すると、コーティング層の表面粗さＲａが大きくなる。そのため、特許文献１では、基材の表面にコーティング層を形成した後、コーティング層の表面を研磨している。 When firing the object to be fired, a firing jig such as a setter is used to place the object to be fired. The firing setter (firing container) of Patent Document 1 has an aluminum or zirconia coating layer formed on the surface of the base material in order to suppress the reaction between the base material and the object to be fired. In Patent Document 1, the particle size of the coating material is adjusted, and as a result, the porosity of the coating layer is adjusted, and peeling between the base material and the coating layer due to the difference in thermal expansion is suppressed. However, if the particle size of the coating material is adjusted in order to suppress the peeling of the coating layer and the base material, the surface roughness Ra of the coating layer becomes large. Therefore, in Patent Document 1, after forming a coating layer on the surface of the base material, the surface of the coating layer is polished.

特開２００７−４５６４１号公報JP-A-2007-45641

特許文献１は、コーティング層の気孔率が大きくなるようにコーティング材の粒径を調整することで基材からのコーティング層の剥離を抑制している。すなわち、大粒径のコーティング材を用いてコーティング層を「疎」にすることによって、基材とコーティング層の熱膨張差を緩和し、コーティング層の剥離を抑制している。その結果、特許文献１は、コーティング層を形成した後の表面研磨が必要となり、製造工程を煩雑にしている。なお、小粒径のコーティング材を用いればコーティング層の表面研磨を省略することが可能となるが、その場合、気孔率が小さくなり、コーティング層の剥離を抑制することができない。そのため、簡易に製造可能であるとともにコーティング層の剥離が抑制された焼成用セッターが必要とされている。本明細書は、従来にない技術的思想に基づき、コーティング層の剥離が抑制された新規な焼成用セッターを提供することを目的とする。 Patent Document 1 suppresses peeling of the coating layer from the base material by adjusting the particle size of the coating material so that the porosity of the coating layer becomes large. That is, by making the coating layer "sparse" by using a coating material having a large particle size, the difference in thermal expansion between the base material and the coating layer is alleviated, and the peeling of the coating layer is suppressed. As a result, Patent Document 1 requires surface polishing after forming the coating layer, which complicates the manufacturing process. If a coating material having a small particle size is used, surface polishing of the coating layer can be omitted, but in that case, the porosity becomes small and peeling of the coating layer cannot be suppressed. Therefore, there is a need for a firing setter that can be easily manufactured and that suppresses peeling of the coating layer. An object of the present specification is to provide a novel firing setter in which peeling of a coating layer is suppressed, based on an unprecedented technical idea.

本発明者らは、基材表面に種々の条件でコーティング層を形成し、コーティング層の剥離性について評価した結果、基材とコーティング層の結合面積がコーティング層の剥離の起こり易さに大きな影響を及ぼしていることを見出した。すなわち、基材とコーティング層の結合面積を所定範囲に調整することにより、基材からのコーティング層の剥離が大幅に抑制されることが判明した。本明細書で開示する焼成用セッターは、上記知見に基づくものである。 As a result of forming a coating layer on the surface of the base material under various conditions and evaluating the peelability of the coating layer, the present inventors have a great influence on the susceptibility of the coating layer to peeling due to the bonding area between the base material and the coating layer. I found that it was exerting. That is, it was found that by adjusting the bonding area between the base material and the coating layer within a predetermined range, peeling of the coating layer from the base material is significantly suppressed. The firing setters disclosed herein are based on the above findings.

本明細書で開示する焼成用セッターは、ＳｉＣとＳｉを主成分とする基材と、基材の表面を被覆しているとともにＺｒ化合物とＡｌ化合物を主成分とするコーティング層を備えていてよい。この焼成用セッターでは、基材とコーティング層の結合面積が、基材表面の面積に対して２０％以上８０％以下であってよい。 The firing setter disclosed in the present specification may include a base material containing SiC and Si as main components, and a coating layer covering the surface of the base material and containing Zr compounds and Al compounds as main components. .. In this firing setter, the bonding area between the base material and the coating layer may be 20% or more and 80% or less with respect to the area of the base material surface.

上記焼成用セッターは、基材とコーティング層の結合面積が２０％以上８０％以下であり、従来の焼成用セッターよりも結合面積が大きい。なお、従来は、基材とコーティング層の結合面積が１０％未満であり、上記焼成用セッターと比較して結合面積が小さい。上記焼成用セッターは、基材とコーティング層の結合面積を大きくすることにより、基材とコーティング層の熱膨張差に基づく両者の剥離を抑制している。また、上記焼成用セッターは、基材とコーティング層の結合面積を調整することによって両者の剥離を抑制しているので、コーティング材の粒径を制限する必要がない。そのため、小粒径のコーティング材を用いることができ、コーティング層を形成した後の研磨を省略することもできる。なお、本明細書でいう「主成分」とは、対象となる部材中に、主成分である材料が５０質量％以上含まれていることを意味する。例えば、「ＳｉＣとＳｉを主成分とする基材」とは、基材中に、ＳｉＣとＳｉの合計が、５０質量％以上含まれていることを意味する。 The firing setter has a bonding area of 20% or more and 80% or less between the base material and the coating layer, and has a larger bonding area than the conventional firing setter. Conventionally, the bonding area between the base material and the coating layer is less than 10%, and the bonding area is smaller than that of the firing setter. The firing setter suppresses the peeling of the base material and the coating layer due to the difference in thermal expansion by increasing the bonding area between the base material and the coating layer. Further, in the firing setter, since the peeling of both is suppressed by adjusting the bonding area between the base material and the coating layer, it is not necessary to limit the particle size of the coating material. Therefore, a coating material having a small particle size can be used, and polishing after forming the coating layer can be omitted. The term "main component" as used herein means that the target member contains 50% by mass or more of the material as the main component. For example, "a base material containing SiC and Si as main components" means that the total amount of SiC and Si is contained in the base material in an amount of 50% by mass or more.

コーティング層は、Ｚｒ化合物を主成分とする表層と、表層と基材の間に設けられているＡｌ化合物を主成分とする中間層を含んでいてよい。この場合、表層は、被焼成物との反応を抑制する反応抑制層として機能する。また、中間層は、表層と基材の間に生じる熱応力（熱膨張差）を緩和する応力緩和層として機能する。コーティング層が表層と中間層を備えることにより、基材からのコーティング層の剥離をより確実に抑制することができる。なお、表層はＺｒ化合物を主成分とし、中間層はＡｌ化合物を主成分とすることにより、ＳｉＣとＳｉを主成分とする基材に対して、熱膨張率が、基材，中間層，表層の順に大きくなる。表層及び中間層を上記材料とすることにより、中間層が応力緩和層として好適に機能する。 The coating layer may include a surface layer containing a Zr compound as a main component and an intermediate layer provided between the surface layer and the base material containing an Al compound as a main component. In this case, the surface layer functions as a reaction suppressing layer that suppresses the reaction with the object to be fired. Further, the intermediate layer functions as a stress relaxation layer that relaxes the thermal stress (thermal expansion difference) generated between the surface layer and the base material. When the coating layer includes a surface layer and an intermediate layer, peeling of the coating layer from the base material can be more reliably suppressed. Since the surface layer contains a Zr compound as a main component and the intermediate layer contains an Al compound as a main component, the coefficient of thermal expansion of the base material containing SiC and Si as the main components is higher than that of the base material, the intermediate layer, and the surface layer. It increases in the order of. By using the surface layer and the intermediate layer as the above materials, the intermediate layer functions suitably as a stress relaxation layer.

中間層は、微量成分としてＦｅ，Ｓｉ，Ｃａ，Ｎａ，Ｍｇ，Ｋの少なくとも１つの元素を含んでいてよい。また、中間層に含まれる微量成分は、中間層の表層側と比較して、中間層の基材側に多く存在していてよい。中間層が微量成分として上記元素を含むことにより、基材と中間層の間にガラス層が形成され易くなり（基材と中間層の接触部分がガラス化し易くなり）、基材と中間層が良好に接合され、両者の接合面積が増大する。なお、本明細書でいう「微量成分」とは、対象となる部材中に含まれる質量が、対象部材の質量に対して３質量％以下であることを意味する。また、「中間層の基材側」とは、中間層の厚み方向（表層と基材を結ぶ方向）における中間層の中央より基材側の範囲のことを意味する。 The intermediate layer may contain at least one element of Fe, Si, Ca, Na, Mg, and K as a trace component. Further, the trace components contained in the intermediate layer may be present in a larger amount on the base material side of the intermediate layer than on the surface layer side of the intermediate layer. When the intermediate layer contains the above element as a trace component, a glass layer is easily formed between the base material and the intermediate layer (the contact portion between the base material and the intermediate layer is easily vitrified), and the base material and the intermediate layer are formed. It is well joined and the joining area of both is increased. The term "trace component" as used herein means that the mass contained in the target member is 3% by mass or less with respect to the mass of the target member. Further, the "base material side of the intermediate layer" means a range from the center of the intermediate layer to the base material side in the thickness direction of the intermediate layer (direction connecting the surface layer and the base material).

上記焼成用セッターでは、コーティング層が表層と中間層を備える場合、表層と中間層の間に、ＡｌとＺｒを含む化合物層が設けられていてもよい。表層と中間層の結合力が増大し、コーティング層の剥離（表層と中間層の剥離）を抑制することができる。 In the above-mentioned firing setter, when the coating layer includes a surface layer and an intermediate layer, a compound layer containing Al and Zr may be provided between the surface layer and the intermediate layer. The bonding force between the surface layer and the intermediate layer is increased, and peeling of the coating layer (peeling of the surface layer and the intermediate layer) can be suppressed.

実施例の焼成用セッターの評価結果を示す。The evaluation result of the firing setter of an Example is shown. 実施例の焼成用セッターのＳＥＭ画像及び元素マッピング画像を示す。The SEM image and the element mapping image of the firing setter of an Example are shown. 比較例の焼成用セッターのＳＥＭ画像及び元素マッピング画像を示す。The SEM image and the element mapping image of the firing setter of the comparative example are shown. 評価試料の取得位置を説明するための模式図を示す。A schematic diagram for explaining the acquisition position of the evaluation sample is shown.

（焼成用セッター）
本明細書で開示する焼成用セッターは、電子部品、セラミック部材等の被焼成物を焼成する際、被焼成物を載置するために用いられる。焼成用セッターの表面（載置面）形状は、三角形，四角形等の多角形であってよく、円形，楕円形等の外縁が曲面を有した形状であってもよい。また、焼成用セッターは、端部（被焼成物を載置する載置部の外側）にリブを備えていてもよい。焼成用セッターは、基材と、基材を被覆しているコーティング層を備えている。 (Baking setter)
The firing setter disclosed in the present specification is used to place the object to be fired when the object to be fired such as an electronic component or a ceramic member is fired. The surface (mounting surface) shape of the firing setter may be a polygon such as a triangle or a quadrangle, or may have a curved outer edge such as a circle or an ellipse. Further, the firing setter may be provided with ribs at the end portion (outside of the mounting portion on which the object to be fired is placed). The firing setter includes a base material and a coating layer covering the base material.

（基材）
基材は、炭化珪素（ＳｉＣ）と珪素（Ｓｉ）を主成分としている。すなわち、ＳｉＣとＳｉの質量の合計が、基材の質量の５０質量％以上を占めている。ＳｉＣとＳｉは、基材中に、６０質量％以上含まれていてよく、７０質量％以上含まれていてよく、８０質量％以上含まれていてよく、９０質量％以上含まれていてよく、９５質量％以上含まれていてよい。基材は、ＳｉＣとＳｉ以外の微量元素を含んでいてよい。微量元素として、鉄（Ｆｅ），カルシウム（Ｃａ），ナトリウム（Ｎａ），マグネシウム（Ｍｇ），カリウム（Ｋ），アルミニウム（Ａｌ）等が挙げられる。各々の微量元素は、基材中に０．０１〜３質量％含まれていてよく、また、基材中の微量元素の合計が０．０１〜３質量％であってよい。なお、基材は、Ｃ粉体，ＳｉＣ粉体及び有機質バインダーを混合・成形した成形体を、金属Ｓｉ存在下で、減圧した不活性ガス雰囲気又は真空中に配置し、成形体中に金属Ｓｉを含浸させて成形することができる。 (Base material)
The base material is mainly composed of silicon carbide (SiC) and silicon (Si). That is, the total mass of SiC and Si accounts for 50% by mass or more of the mass of the base material. SiC and Si may be contained in the base material in an amount of 60% by mass or more, 70% by mass or more, 80% by mass or more, and 90% by mass or more. It may be contained in an amount of 95% by mass or more. The base material may contain trace elements other than SiC and Si. Examples of trace elements include iron (Fe), calcium (Ca), sodium (Na), magnesium (Mg), potassium (K), aluminum (Al) and the like. Each trace element may be contained in the base material in an amount of 0.01 to 3% by mass, and the total amount of the trace elements in the base material may be 0.01 to 3% by mass. As the base material, a molded body obtained by mixing and molding C powder, SiC powder and an organic binder is placed in a depressurized inert gas atmosphere or vacuum in the presence of metal Si, and the metal Si is placed in the molded body. Can be impregnated and molded.

（コーティング層）
コーティング層は、基材の表面を被覆している。すなわち、コーティング層は、焼成用セッターの表面に露出している。コーティング層は、焼成用セッターの全面を被覆していてもよいし、焼成用セッターの表面（被焼成物を載置する面）のみを被覆していてもよい。コーティング層は、基材表面にコーティング材を塗布した後、１１００〜１４００度で焼成して基材表面に固着させてよい。コーティング材を塗布した後の焼成温度は、１２００度以上であってよく、１２４０度以上であってよく、１３００度以上であってよい。コーティング層は、ジルコニウム（Ｚｒ）化合物とアルミニウム（Ａｌ）化合物を主成分としている。すなわち、Ｚｒ化合物とＡｌ化合物の質量の合計が、コーティング層の質量の５０質量％以上を占めている。Ｚｒ化合物とＡｌ化合物は、コーティング層中に、６０質量％以上含まれていてよく、７０質量％以上含まれていてよく、８０質量％以上含まれていてよく、９０質量％以上含まれていてよく、９５質量％以上含まれていてよい。コーティング層は、Ｚｒ化合物とＡｌ化合物以外の微量元素を含んでいてよい。すなわち、コーティング層内に、Ｚｒ化合物とＡｌ化合物以外の元素が３質量％以下含まれていてもよい。微量元素として、Ｆｅ，Ｓｉ，Ｃａ，Ｎａ，Ｍｇ，Ｋ等が挙げられ、コーティング層内にこれらの元素が１つ以上含まれていてよい。 (Coating layer)
The coating layer covers the surface of the base material. That is, the coating layer is exposed on the surface of the firing setter. The coating layer may cover the entire surface of the firing setter, or may cover only the surface of the firing setter (the surface on which the object to be fired is placed). The coating layer may be fixed to the surface of the base material by applying a coating material to the surface of the base material and then firing at 1100 to 1400 degrees. The firing temperature after applying the coating material may be 1200 ° C. or higher, 1240 ° C. or higher, or 1300 ° C. or higher. The coating layer is mainly composed of a zirconium (Zr) compound and an aluminum (Al) compound. That is, the total mass of the Zr compound and the Al compound accounts for 50% by mass or more of the mass of the coating layer. The Zr compound and the Al compound may be contained in the coating layer in an amount of 60% by mass or more, 70% by mass or more, 80% by mass or more, and 90% by mass or more. It may be contained in an amount of 95% by mass or more. The coating layer may contain trace elements other than Zr compounds and Al compounds. That is, the coating layer may contain 3% by mass or less of elements other than the Zr compound and the Al compound. Examples of the trace element include Fe, Si, Ca, Na, Mg, K and the like, and one or more of these elements may be contained in the coating layer.

コーティング層は、基材の表面と結合している。基材とコーティング層の結合面積は、基材表面の面積に対して２０％以上８０％以下であってよい。基材とコーティング層の結合面積は、４０％以上であってよく、５０％以上であってよく、６０％以上であってよい。また、コーティング層は、組成が異なる表層と中間層を備えていてよい。 The coating layer is bonded to the surface of the substrate. The bonding area between the base material and the coating layer may be 20% or more and 80% or less with respect to the area of the base material surface. The bonding area between the base material and the coating layer may be 40% or more, 50% or more, and 60% or more. Further, the coating layer may include a surface layer and an intermediate layer having different compositions.

（表層）
表層は、焼成用セッターの露出面であってよい。すなわち、表層は、被焼成物と接触する接触面を構成していてよい。表層の主成分は、Ｚｒ化合物であってよい。Ｚｒ化合物は、表層中に、５０質量％以上含まれていてよく、６０質量％以上含まれていてよく、７０質量％以上含まれていてよく、８０質量％以上含まれていてよく、９０質量％以上含まれていてよく、９５質量％以上含まれていてよい。Ｚｒ化合物として、カルシア（ＣａＯ）またはイットリア（Ｙ２Ｏ３）で安定化された安定化ジルコニア、アルミナとジルコニアの共晶物、ＢａＺｒＯ３、ＣａＺｒＯ３等が挙げられる。表層の厚みは、１０〜１００μｍであってよい。表層の厚みは、２０μｍ以上であってよく、３０μｍ以上であってよく、４０μｍ以上であってよく、５０μｍ以上であってよい。また、表層の厚みは、９０μｍ以下であってよく、８０μｍ以下であってよく、７０μｍ以下であってよい。 (surface)
The surface layer may be an exposed surface of the firing setter. That is, the surface layer may form a contact surface that comes into contact with the object to be fired. The main component of the surface layer may be a Zr compound. The Zr compound may be contained in the surface layer in an amount of 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, and 90% by mass. It may be contained in an amount of% or more, and may be contained in an amount of 95% by mass or more. As Zr compound, calcia (CaO) or yttria (Y 2 O 3) stabilized with stabilized zirconia, alumina and zirconia eutectic, BaZrO 3, CaZrO 3, and the like. The thickness of the surface layer may be 10 to 100 μm. The thickness of the surface layer may be 20 μm or more, 30 μm or more, 40 μm or more, and 50 μm or more. The thickness of the surface layer may be 90 μm or less, 80 μm or less, and 70 μm or less.

（中間層）
中間層は、表層と基材の間に設けられていてよい。中間層は、表層及び基材に接合していてよい。すなわち、中間層が、表層と基材を接合していてよい。中間層の主成分は、Ａｌ化合物であってよい。Ａｌ化合物は、中間層中に、５０質量％以上含まれていてよく、６０質量％以上含まれていてよく、７０質量％以上含まれていてよく、８０質量％以上含まれていてよく、９０質量％以上含まれていてよく、９５質量％以上含まれていてよい。Ａｌ化合物として、ムライト（アルミニウムシリケート）が挙げられる。中間層の厚みは、５０〜２００μｍであってよい。中間層の厚みは、６０μｍ以上であってよく、７０μｍ以上であってよく、８０μｍ以上であってよく、１００μｍ以上であってよい。また、中間層の厚みは、１８０μｍ以下であってよく、１６０μｍ以下であってよい。中間層の厚みは、表層の厚みより厚くてよい。 (Middle layer)
The intermediate layer may be provided between the surface layer and the base material. The intermediate layer may be bonded to the surface layer and the base material. That is, the intermediate layer may join the surface layer and the base material. The main component of the intermediate layer may be an Al compound. The Al compound may be contained in the intermediate layer in an amount of 50% by mass or more, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more. It may be contained in an amount of 95% by mass or more, and may be contained in an amount of 95% by mass or more. Examples of the Al compound include mullite (aluminum silicate). The thickness of the intermediate layer may be 50 to 200 μm. The thickness of the intermediate layer may be 60 μm or more, 70 μm or more, 80 μm or more, and 100 μm or more. The thickness of the intermediate layer may be 180 μm or less, and may be 160 μm or less. The thickness of the intermediate layer may be thicker than the thickness of the surface layer.

コーティング層が表層と中間層を備える場合、上記した微量成分（Ｆｅ，Ｓｉ，Ｃａ，Ｎａ，Ｍｇ，Ｋ等）は、中間層に含まれていてよい。また、中間層に含まれる微量成分は、基材側に偏在していてよい。すなわち、微量成分は、中間層の表層側（中間層の厚み方向中央よりも表層側の範囲）と比較して、中間層の基材側（中間層の厚み方向中央よりも基材側の範囲）に多く存在してよい。微量成分は、基材，中間層に含まれるＳｉ原料のガラス化を促進させ、基材と中間層の結合面積を増大させることに寄与する。 When the coating layer includes a surface layer and an intermediate layer, the above-mentioned trace components (Fe, Si, Ca, Na, Mg, K, etc.) may be contained in the intermediate layer. Further, the trace components contained in the intermediate layer may be unevenly distributed on the base material side. That is, the trace components are in the range of the base material side of the intermediate layer (the range of the base material side of the center of the intermediate layer in the thickness direction) as compared with the surface layer side of the intermediate layer (the range of the surface layer side of the middle layer in the thickness direction). ) May be present in large numbers. The trace component promotes the vitrification of the Si raw material contained in the base material and the intermediate layer, and contributes to increasing the bonding area between the base material and the intermediate layer.

コーティング層が表層と中間層を備える場合、表層と中間層の間に、ＡｌとＺｒを含む化合物層が設けられていてよい。すなわち、表層と中間層の間に、Ｚｒ化合物を主成分とする表層と、Ａｌ化合物を主成分とする中間層が反応した反応層が設けられていてよい。反応層は、表層と中間層の剥離を抑制することに寄与する。なお、基材の表面に中間層，表層を形成した後に焼成を行い、コーティング層（表層及び中間層）を基材表面に固着させてよい。あるいは、表面に中間層を形成した後に焼成を行って基材表面に中間層を固着させた後、中間層の表面に表層を形成して再度焼成を行ってもよい。 When the coating layer includes a surface layer and an intermediate layer, a compound layer containing Al and Zr may be provided between the surface layer and the intermediate layer. That is, a reaction layer in which a surface layer containing a Zr compound as a main component and an intermediate layer containing an Al compound as a main component react may be provided between the surface layer and the intermediate layer. The reaction layer contributes to suppressing the peeling of the surface layer and the intermediate layer. After forming the intermediate layer and the surface layer on the surface of the base material, firing may be performed to fix the coating layer (surface layer and the intermediate layer) to the surface of the base material. Alternatively, after forming the intermediate layer on the surface and firing to fix the intermediate layer on the surface of the base material, a surface layer may be formed on the surface of the intermediate layer and firing may be performed again.

（評価方法）
基材とコーティング層の結合面積の測定位置、及び、結合面積の算出方法について説明する。図４は、焼成用セッターの一例として、四角形（正方形）の焼成用セッター１０を示している。基材とコーティング層の結合面積の測定は、コーティング層の状態が標準的である位置について行う。すなわち、結合面積の測定は、コーティング層の状態が特異な状態となる可能性がある位置を避けて行う。具体的には、焼成用セッター１０の側面１２から距離Ｄ１２の位置に測定領域１４を設定し、焼成用セッター１０の重心２０（図４の場合、焼成用セッター１０の中心と同一）から最も離れた位置にある測定領域１４を遠方部１４ａと設定し、重心２０と遠方部１４ａの中点を測定位置２２とする。焼成用セッター１０の場合、測定位置２２が４箇所存在する。なお、焼成用セッターの形状が、四角形以外の多角形、円形，楕円形等の外縁が曲面を有した形状であっても、同様の方法で測定位置を決定する。なお、距離Ｄ１２は、焼成用セッターの重心から側面までの距離が５０ｍｍ以上の場合は２０ｍｍとする。また、重心から側面までの距離が５０ｍｍ未満の場合は、距離Ｄ１２は、重心から側面までの距離の２０％とする。 (Evaluation method)
The measurement position of the bonding area between the base material and the coating layer and the calculation method of the bonding area will be described. FIG. 4 shows a square (square) firing setter 10 as an example of the firing setter. The measurement of the bonding area between the base material and the coating layer is performed at a position where the state of the coating layer is standard. That is, the measurement of the bonding area is performed while avoiding a position where the state of the coating layer may be a peculiar state. Specifically, the measurement region 14 is set at a position of a distance D12 from the side surface 12 of the firing setter 10, and is farthest from the center of gravity 20 of the firing setter 10 (in the case of FIG. 4 , it is the same as the center of the firing setter 10). The measurement region 14 at the above position is set as the distant portion 14a, and the midpoint between the center of gravity 20 and the distant portion 14a is set as the measurement position 22. In the case of the firing setter 10, there are four measurement positions 22. Even if the shape of the firing setter is a polygon other than a quadrangle, a circle, an ellipse, or the like having a curved outer edge, the measurement position is determined by the same method. The distance D12 is 20 mm when the distance from the center of gravity of the firing setter to the side surface is 50 mm or more. When the distance from the center of gravity to the side surface is less than 50 mm, the distance D12 is 20% of the distance from the center of gravity to the side surface.

基材とコーティング層の結合面積は、上記した測定位置（図４の測定位置２２を参照）で焼成用セッターを切断し、その切断面を観察し、基材の表面長さに対する基材とコーティング層が接合している部分の長さの割合から算出する。例えば、図２に示すように、焼成用セッターのＳＥＭ（Scanning Electron Microscope）画像を取得し、基材表面の長さを測定し、基材と中間層が結合している結合部分の長さを測定し、下記式（１）より結合面積を算出する。
結合面積＝（結合部分の長さ）／（基材表面の長さ）×１００・・・（１） For the bonding area between the base material and the coating layer, cut the firing setter at the above-mentioned measurement position (see the measurement position 22 in FIG. 4 ), observe the cut surface, and observe the cut surface of the base material and the coating with respect to the surface length of the base material. It is calculated from the ratio of the length of the part where the layers are joined. For example, as shown in FIG. 2, an SEM (Scanning Electron Microscope) image of a firing setter is acquired, the length of the surface of the base material is measured, and the length of the bonded portion where the base material and the intermediate layer are bonded is determined. The measurement is performed, and the bonding area is calculated from the following formula (1).
Bonded area = (length of bonded portion) / (length of substrate surface) x 100 ... (1)

基材表面に種々の条件でコーティング層を形成して焼成用セッターを製作し、製作した焼成用セッターについて繰り返し加熱試験を実施し、コーティング層の状態（剥離・膨れの有無）について評価した。 A coating layer was formed on the surface of the base material under various conditions to produce a firing setter, and the produced firing setter was repeatedly subjected to a heating test to evaluate the state of the coating layer (presence or absence of peeling / swelling).

図１に、実施例で用いた試料の特徴、及び、繰り返し加熱試験の結果を示す。実施例で用いた試料は、Ｓｉ−ＳｉＣ質の基材表面にスプレーコート法を用いてコーティング層を形成し、図１に示す温度で２時間焼成することにより製作した。なお、コーティング材は、平均粒径１００μｍの原料をポットミルを用いて粉砕し、１０〜２０μｍに調整した。実施例１〜５は、基材とコーティング層の結合面積を増大させるため、コーティング材（コーティング用スラリー）に焼結助剤を図１に示す割合で添加した。焼結助剤として、Ｎａ，Ｃａ，Ｍｇ，Ｆｅ，Ｓｉ等を含む市販の焼結助剤を用いた。なお、実施例３と４は、焼成温度のみが異なる。また、比較例として、コーティング材に焼結助剤を添加しないでコーティング層を形成し、図１に示す温度で２時間焼成した試料（比較例１〜３）を製作した。 FIG. 1 shows the characteristics of the sample used in the examples and the results of the repeated heating test. The sample used in the examples was produced by forming a coating layer on the surface of a SiC-material substrate by a spray coating method and firing at the temperature shown in FIG. 1 for 2 hours. The coating material was adjusted to 10 to 20 μm by pulverizing a raw material having an average particle size of 100 μm using a pot mill. In Examples 1 to 5, in order to increase the bonding area between the base material and the coating layer, a sintering aid was added to the coating material (coating slurry) at the ratio shown in FIG. As the sintering aid, a commercially available sintering aid containing Na, Ca, Mg, Fe, Si and the like was used. In addition, only the firing temperature is different between Examples 3 and 4. Further, as a comparative example, a sample (Comparative Examples 1 to 3) was produced in which a coating layer was formed without adding a sintering aid to the coating material and baked at the temperature shown in FIG. 1 for 2 hours.

繰り返し加熱試験は、各試料を昇温速度１００℃／時間で１３５０℃まで加熱し、１３５０℃で２時間保持し、その後室温まで自然冷却する工程を１サイクルとし、５サイクル実施した。各サイクル終了後、焼成用セッターの外観を観察し、コーティング層の剥離・膨れの有無を評価した。コーティング層の剥離・膨れが全く確認されなかったものを「Ａ」とし、剥離・膨れは観察されなかったものの剥離・膨れの兆しがあるものを「Ｂ」とし、剥離・膨れが確認されたものを「Ｃ」とし、図１に示す。 In the repeated heating test, each sample was heated to 1350 ° C. at a heating rate of 100 ° C./hour, held at 1350 ° C. for 2 hours, and then naturally cooled to room temperature as one cycle, and 5 cycles were carried out. After the end of each cycle, the appearance of the firing setter was observed, and the presence or absence of peeling and swelling of the coating layer was evaluated. Those in which no peeling / swelling was confirmed in the coating layer were designated as "A", those in which no peeling / swelling was observed but in which there were signs of peeling / swelling were designated as "B", and those in which peeling / swelling was confirmed. Is "C" and is shown in FIG.

図１に示すように、基材とコーティング層の接合面積が２０％以上８０％以下の試料（実施例１〜５）は、繰り返し加熱試験を５サイクル実施しても、コーティング層の剥離・膨れが確認されなかった。一方、接合面積が２０％未満の試料（比較例１〜３）は、いずれも１サイクル終了時にコーティング層の剥離・膨れが確認された。なお、本実施例では差異が確認できなかったが、基材上におけるコーティング層の状態がばらつく可能性（塗装ムラの発生等）を考慮すると、接合面積は４０％（４３％）以上であることが好ましい。また、コーティング層を基材に固着させるときの焼き付けムラ（焼成ムラ）が生じる可能性を考慮すると、接合面積は５０％（５２％）以上であることが好ましい。また、コーティング層中の不純物（結合助剤）を抑制するという観点より、接合面積は６０％以下であることが好ましい。 As shown in FIG. 1, in the samples (Examples 1 to 5) in which the bonding area between the base material and the coating layer is 20% or more and 80% or less, the coating layer is peeled off and swollen even after repeated heating tests are performed for 5 cycles. Was not confirmed. On the other hand, in all the samples having a bonding area of less than 20% (Comparative Examples 1 to 3), peeling and swelling of the coating layer was confirmed at the end of one cycle. Although no difference could be confirmed in this example, the joint area should be 40% (43%) or more in consideration of the possibility that the state of the coating layer on the substrate varies (occurrence of coating unevenness, etc.). Is preferable. Further, considering the possibility of baking unevenness (baking unevenness) when the coating layer is fixed to the base material, the bonding area is preferably 50% (52%) or more. Further, from the viewpoint of suppressing impurities (binding aids) in the coating layer, the bonding area is preferably 60% or less.

また、実施例１及び比較例３の試料について測定部分２２（図４も参照）の断面のＳＥＭ画像を取得し、ＥＰＭＡ（Electron Probe Micro Analyzer）を用いて断面の元素分析を行った。図２は実施例１の試料の結果を示し、図３は比較例３の試料の結果を示している。なお、図２及び図３には、Ｎａ，Ｓｉ，Ｃａ，Ｙ及びＺｒのマッピングデータを示している。 In addition, SEM images of the cross section of the measurement portion 22 (see also FIG. 4) were acquired for the samples of Example 1 and Comparative Example 3, and elemental analysis of the cross section was performed using EPMA (Electron Probe Micro Analyzer). FIG. 2 shows the results of the sample of Example 1, and FIG. 3 shows the results of the sample of Comparative Example 3. Note that FIGS. 2 and 3 show mapping data of Na, Si, Ca, Y and Zr.

ＳＥＭ画像から明らかなように、実施例１の焼成用セッターは、比較例３の焼成用セッターよりも基材とコーティング層（中間層）がよく接合している（接合面積が大きい）。また、実施例１の中間層に含まれる元素に着目すると、焼結助剤に由来するＮａ，Ｓｉ，Ｃａといった微量元素が、中間層の表層側と比較して、中間層の基材側に多く存在していることが確認された（図２）。より具体的には、微量元素が、中間層と基材の界面に偏在している。一方、図３に示すように、比較例３の焼成用セッターは、中間層と基材の界面に微量元素が確認されない。中間層と基材の界面に微量元素が偏在している焼成用セッター（実施例１）は、基材と中間層の接合面積が大きく、耐久性が高いことが確認された。 As is clear from the SEM image, in the firing setter of Example 1, the base material and the coating layer (intermediate layer) are bonded better (the bonding area is larger) than that of the firing setter of Comparative Example 3. Focusing on the elements contained in the intermediate layer of Example 1, trace elements such as Na, Si, and Ca derived from the sintering aid are located on the base material side of the intermediate layer as compared with the surface layer side of the intermediate layer. It was confirmed that there were many (Fig. 2). More specifically, trace elements are unevenly distributed at the interface between the intermediate layer and the base material. On the other hand, as shown in FIG. 3, in the firing setter of Comparative Example 3, trace elements are not confirmed at the interface between the intermediate layer and the base material. It was confirmed that the firing setter (Example 1) in which trace elements are unevenly distributed at the interface between the intermediate layer and the base material has a large bonding area between the base material and the intermediate layer and has high durability.

また、中間層と基材の界面の微量元素の偏在が結合面積に影響を与えることは、図１に示す結果からも確認される。図１に示すように、焼結助剤の添加量が増えるに従って、基材と中間層の結合面積が増大している（実施例１，２，４，５及び比較例３）。なお、焼成温度を上昇させることによっても、基材と中間層の結合面積が増大することが確認される（実施例３と４、比較例１〜３）。しかしながら、図１に示す結果より、焼成温度の変化が結合面積に与える影響と比べ、微量元素（焼結助剤）の添加量の変化が結合面積に与える影響の方が大きいことが確認される。 It is also confirmed from the results shown in FIG. 1 that the uneven distribution of trace elements at the interface between the intermediate layer and the base material affects the bonding area. As shown in FIG. 1, as the amount of the sintering aid added increases, the bonding area between the base material and the intermediate layer increases (Examples 1, 2, 4, 5 and Comparative Example 3). It is confirmed that the bonding area between the base material and the intermediate layer is also increased by increasing the firing temperature (Examples 3 and 4, Comparative Examples 1 to 3). However, from the results shown in FIG. 1, it is confirmed that the effect of the change in the amount of the trace element (sintering aid) added on the bond area is larger than the effect of the change in the firing temperature on the bond area. ..

また、図２に示すように、中間層の表層側に着目すると、実施例１の焼成用セッターでは、表層に特有の元素（Ｙ，Ｚｒ）が中間層の表層側（中間層と表層の界面）に存在していることが確認された（図３も比較参照）。すなわち、実施例１の焼成用セッターは、表層と中間層の間に、中間層に由来するＡｌと表層に由来するＹ及びＺｒとを含む化合物が形成されていることが確認された。換言すると、実施例１の焼成用セッターは、表層と中間層の界面に、両層に含まれる元素を含む化合物が形成されていることが確認された。この結果は、実施例１の焼成用セッターは表層と中間層が強固に接合され、中間層から表層が剥離し難くなっていることを示している。すなわち、実施例１の焼成用セッターでは、被焼成物との反応を抑制する表層が、焼成用セッターから剥離することを抑制することができることを示している。 Further, as shown in FIG. 2, focusing on the surface layer side of the intermediate layer, in the firing setter of Example 1, the elements (Y, Zr) peculiar to the surface layer are on the surface layer side of the intermediate layer (the interface between the intermediate layer and the surface layer). ) Was confirmed (see also comparison in FIG. 3). That is, in the firing setter of Example 1, it was confirmed that a compound containing Al derived from the intermediate layer and Y and Zr derived from the surface layer was formed between the surface layer and the intermediate layer. In other words, in the firing setter of Example 1, it was confirmed that a compound containing the elements contained in both layers was formed at the interface between the surface layer and the intermediate layer. This result indicates that in the firing setter of Example 1, the surface layer and the intermediate layer are firmly bonded, and the surface layer is difficult to peel off from the intermediate layer. That is, in the firing setter of Example 1, it is shown that the surface layer that suppresses the reaction with the object to be fired can be suppressed from peeling from the firing setter.

以上、本発明の具体例を詳細に説明したが、これらは例示に過ぎず、特許請求の範囲を限定するものではない。特許請求の範囲に記載の技術には、以上に例示した具体例を様々に変形、変更したものが含まれる。また、本明細書または図面に説明した技術要素は、単独であるいは各種の組合せによって技術的有用性を発揮するものであり、出願時請求項記載の組合せに限定されるものではない。また、本明細書または図面に例示した技術は複数目的を同時に達成し得るものであり、そのうちの一つの目的を達成すること自体で技術的有用性を持つものである。 Although specific examples of the present invention have been described in detail above, these are merely examples and do not limit the scope of claims. The techniques described in the claims include various modifications and modifications of the specific examples illustrated above. In addition, the technical elements described in the present specification or the drawings exhibit technical usefulness alone or in various combinations, and are not limited to the combinations described in the claims at the time of filing. In addition, the techniques illustrated in the present specification or drawings can achieve a plurality of purposes at the same time, and achieving one of the purposes itself has technical usefulness.

Claims (3)

ＳｉＣとＳｉを主成分とする基材と、
基材の表面を被覆しているとともにＺｒ化合物とＡｌ化合物を主成分とするコーティング層と、
を備えており、
コーティング層は、Ｚｒ化合物を主成分とする表層と、表層と基材の間に設けられているＡｌ化合物を主成分とする中間層と、を含んでおり、
基材とコーティング層の結合面積が、基材表面の面積に対して２０％以上８０％以下である焼成用セッター。 A base material containing SiC and Si as the main components,
A coating layer that covers the surface of the base material and contains Zr compounds and Al compounds as main components,
Is equipped with
The coating layer includes a surface layer containing a Zr compound as a main component and an intermediate layer provided between the surface layer and the base material containing an Al compound as a main component.
A firing setter in which the bonding area between the base material and the coating layer is 20% or more and 80% or less with respect to the area of the base material surface. 中間層は、微量成分としてＦｅ，Ｓｉ，Ｃａ，Ｎａ，Ｍｇ，Ｋの少なくとも１つの元素を含み、
前記微量成分は、中間層の前記表層側と比較して、中間層の基材側に多く存在している請求項１に記載の焼成用セッター。 The intermediate layer contains at least one element of Fe, Si, Ca, Na, Mg, and K as a trace component, and contains at least one element.
The firing setter according to claim 1 , wherein the trace components are present in a larger amount on the base material side of the intermediate layer than on the surface layer side of the intermediate layer. 表層と中間層の間に、ＡｌとＺｒを含む化合物層が設けられている請求項１又は２に記載の焼成用セッター。 The firing setter according to claim 1 or 2 , wherein a compound layer containing Al and Zr is provided between the surface layer and the intermediate layer.
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