JP2009062243A - Recycling method for firing containers - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000004064 recycling Methods 0.000 title 1
- 239000000463 material Substances 0.000 claims abstract description 40
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- 239000000758 substrate Substances 0.000 claims abstract description 28
- 230000001172 regenerating effect Effects 0.000 claims abstract description 18
- 238000011069 regeneration method Methods 0.000 claims abstract description 12
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 9
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- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000008929 regeneration Effects 0.000 claims abstract description 7
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Abstract
【課題】多孔質ＳｉＣ質基材を用いた焼成用容器の再生に適し、安価な焼成用容器の再生方法を提供する。
【解決手段】本焼成用容器の再生方法は、見かけ気孔率が１５％以上、曲げ強さが３５ＭＰａ以上である多孔質ＳｉＣ質基材の少なくとも被焼成物を載置する部分の表面に、Ａｌ２Ｏ３、ＺｒＯ２、ムライト、ジルコンの少なくとも１種または複数を主成分とするセラミックス皮膜を形成した焼成用容器を、数回使用した後に、多孔質ＳｉＣ質基材の表面に形成されていたセラミックス皮膜を除去し、上記同様のセラミックス皮膜を厚さ３０〜５００μｍ形成し、再生する。
【選択図】 なしAn object of the present invention is to provide an inexpensive method for regenerating a firing container that is suitable for the regeneration of a firing container using a porous SiC substrate.
A method for regenerating a firing container includes a surface of a porous SiC substrate having an apparent porosity of 15% or more and a bending strength of 35 MPa or more. It was formed on the surface of the porous SiC base material after using a firing container in which a ceramic film mainly composed of at least one or more of 2 O 3 , ZrO 2 , mullite, and zircon was used several times. The ceramic film is removed, and a ceramic film similar to the above is formed to a thickness of 30 to 500 μm and regenerated.
[Selection figure] None
Description
本発明は焼成用容器の再生方法に係り、特に多孔質ＳｉＣ質基材を用いる焼成用容器の再生方法に関する。 The present invention relates to a method for regenerating a firing container, and more particularly to a method for regenerating a firing container using a porous SiC substrate.
従来、セラミック電子部品の焼成は、一般に１０００〜１７００℃の温度域で熱処理または焼成が行われる。 Conventionally, firing of ceramic electronic components is generally performed by heat treatment or firing in a temperature range of 1000 to 1700 ° C.
このため、電子部品用セラミックスの焼成用容器としては、Ａｌ２Ｏ３−ＳｉＯ２質、Ａｌ２Ｏ３−ＳｉＯ２質−ＭｇＯ質、ＭｇＯ質−Ａｌ２Ｏ３−ＺｒＯ２質、ＳｉＣ質等の耐熱性に優れたセラミックスが用いられる。この中でも特に、ＳｉＣ質セラミックスは、耐熱強度及び耐クリープ性に優れているため、好適な材料であるとされている（特許文献１）。 For this reason, Al 2 O 3 —SiO 2 quality, Al 2 O 3 —SiO 2 quality—MgO quality, MgO quality—Al 2 O 3 —ZrO 2 quality, SiC quality, etc. Ceramics with excellent heat resistance are used. Among these, in particular, SiC ceramics are considered to be suitable materials because they are excellent in heat resistance and creep resistance (Patent Document 1).
しかしながら、特許文献１の焼成用容器は、使用中に基材自体が割れたり、反ったりすることは稀であるが、皮膜剥離あるいは被焼成品との反応により再使用が不可能になることがある。再使用不可能になった焼成用容器は、基材自体の再使用は可能であり、廃棄するのは、焼成用容器を用いた焼成コストの低減及び廃棄物低減の観点からも好ましくない。 However, the firing container of Patent Document 1 rarely breaks or warps the substrate itself during use, but may not be reusable due to film peeling or reaction with the fired product. is there. The firing container that has become non-reusable can reuse the base material itself, and it is not preferable to discard the base material from the viewpoints of reducing the firing cost and reducing the waste using the firing container.
そこで、特許文献２に記載の発明のように、焼成用容器を再利用するのが好ましい。 Therefore, it is preferable to reuse the firing container as in the invention described in Patent Document 2.
特許文献２に記載の焼成用容器の再生方法は、ＳｉＣ９７％、見掛気孔率が０％のような緻密質ＳｉＣ質基材の表面にＡｌ２Ｏ３、ムライト、ＺｒＯ２、スピネルの少なくとも１種または複数を主成分とするセラミックス被膜を形成した焼成用容器の再生方法において、この焼成用容器を数回使用した後に、緻密質ＳｉＣ質基材の表面にセラミックス被膜を３０〜５００μｍプラズマ溶射し、再生する方法である。 In the method for regenerating the firing container described in Patent Document 2, at least one of Al 2 O 3 , mullite, ZrO 2 , and spinel is formed on the surface of a dense SiC substrate having a SiC of 97% and an apparent porosity of 0%. In a method for regenerating a firing container in which a ceramic film mainly composed of seeds or plural is formed, after the firing container is used several times, the ceramic film is plasma sprayed on the surface of the dense SiC substrate by 30 to 500 μm. , How to play.
このような再生方法では、緻密質ＳｉＣ質基材を用いた焼成用容器の再生には適するが、多孔質ＳｉＣ質基材を用いた焼成用容器の再生には適さない。また、皮膜を除去再生するためには、皮膜除去後のＳｉＣ質基材表面の表面粗さが３〜１５μｍ程度である必要があるが、用途によってはＳｉＣ質表面の凸部が酸化、さらに被焼成物成分との反応により強度が低下し皮膜を除去すると十分な表面粗さが得られない場合がある。 Such a regeneration method is suitable for regeneration of a firing container using a dense SiC substrate, but is not suitable for regeneration of a firing container using a porous SiC substrate. In addition, in order to remove and regenerate the film, the surface roughness of the SiC substrate surface after removal of the film needs to be about 3 to 15 μm. When the strength is lowered by the reaction with the fired product component and the film is removed, a sufficient surface roughness may not be obtained.
再度の粗面化処理はＳｉＣの硬度が非常に高いためにブラスト等の機械的な粗面化方法では対応は難しい。ケミカルエッチング等を用いれば可能であるが、使用後の基材は表面の強度低下、被焼成物成分の浸透等がありその程度は製品の使用履歴によって異なってくる。一定条件では安定した粗面化面を得ることは難しく、基材の使用状況に応じてエッチング条件を調整しなくてはならないため高コストとなる。
本発明は上述した事情を考慮してなされたもので、多孔質ＳｉＣ質基材を用いた焼成用容器の再生に適し、安価な焼成用容器の再生方法を提供することを目的とする。 The present invention has been made in consideration of the above-described circumstances, and an object thereof is to provide an inexpensive method for regenerating a firing container that is suitable for the regeneration of a firing container using a porous SiC base material.
上述した目的を達成するため、本発明に係る焼成用容器の再生方法は、セラミックス部品の被焼成物を載置して用い、見かけ気孔率が１５％以上であり、かつ、曲げ強さが３５ＭＰａ以上である多孔質ＳｉＣ質基材の少なくとも前記被焼成物を載置する部分の表面に、Ａｌ２Ｏ３、ＺｒＯ２、ムライト（Ａｌ２Ｏ３−ＳｉＯ２）、ジルコン（ＺｒＳｉＯ４）の少なくとも１種または複数を主成分とするセラミックス皮膜を形成した焼成用容器を、数回使用した後に、前記多孔質ＳｉＣ質基材の前記表面に形成されていた前記セラミックス皮膜を除去し、新たにＡｌ２Ｏ３、ＺｒＯ２、ムライト、ジルコンの少なくとも１種または複数を主成分とするセラミックス皮膜を厚さ３０〜５００μｍ形成し、再生することを特徴とする。 In order to achieve the above-described object, the method for regenerating a firing container according to the present invention uses a ceramic part fired material, has an apparent porosity of 15% or more, and a bending strength of 35 MPa. On the surface of at least the portion on which the object to be fired is placed on the porous SiC base material, at least Al 2 O 3 , ZrO 2 , mullite (Al 2 O 3 —SiO 2 ), zircon (ZrSiO 4 ) After using the firing container on which the ceramic film mainly composed of one or more is used several times, the ceramic film formed on the surface of the porous SiC base material is removed, and a new Al A ceramic film mainly composed of at least one or more of 2 O 3 , ZrO 2 , mullite, and zircon is formed to a thickness of 30 to 500 μm and regenerated.
本発明に係る焼成用容器の再生方法によれば、多孔質ＳｉＣ質基材を用いた焼成用容器の再生に適し、安価な焼成用容器の再生方法を提供することができる。 According to the method for regenerating a firing container according to the present invention, it is possible to provide an inexpensive method for regenerating a firing container that is suitable for regeneration of a firing container using a porous SiC base material.
本発明の一実施形態に係る焼成用容器の再生方法を説明する。 A method for regenerating a firing container according to an embodiment of the present invention will be described.
本発明の一実施形態に係る焼成用容器の再生方法は、セラミックス部品の被焼成物を載置して用いる基材は、見かけ気孔率が１５％以上、曲げ強さが３５ＭＰａ以上である多孔質ＳｉＣ質基材が対象であり、多孔質ＳｉＣ質基材の少なくとも被焼成物を載置する部分の表面に、Ａｌ２Ｏ３、ＺｒＯ２、ムライト（Ａｌ２Ｏ３−ＳｉＯ２）、ジルコン（ＺｒＳｉＯ４）の少なくとも１種または複数を主成分とするセラミックス皮膜を形成した焼成用容器を、数回使用した後に、多孔質ＳｉＣ質基材の表面に形成されていたセラミックス皮膜を除去し、新たにＡｌ２Ｏ３、ＺｒＯ２、ムライト、ジルコンの少なくとも１種または複数を主成分とするセラミックス皮膜を厚さ３０〜５００μｍ形成し、再生する。 In the method for reclaiming a firing container according to an embodiment of the present invention, the substrate used by placing the ceramic part firing object is a porous material having an apparent porosity of 15% or more and a bending strength of 35 MPa or more. The SiC base material is the target, and at least the surface of the porous SiC base material on which the object to be fired is placed is Al 2 O 3 , ZrO 2 , mullite (Al 2 O 3 —SiO 2 ), zircon ( ZrSiO 4 ) After firing the firing container on which a ceramic film mainly composed of at least one or more of ZrSiO 4 ) is used several times, the ceramic film formed on the surface of the porous SiC substrate is removed, and a new A ceramic film mainly composed of at least one or more of Al 2 O 3 , ZrO 2 , mullite and zircon is formed to a thickness of 30 to 500 μm and regenerated.
一般に、セラミック電子部品の焼成は１０００〜１７００℃で行われる。 Generally, firing of ceramic electronic components is performed at 1000 to 1700 ° C.
焼成用容器としては、Ａｌ２Ｏ３、Ａｌ２Ｏ３−ＳｉＯ２、Ａｌ２Ｏ３・ＳｉＯ２・ＭｇＯ、Ａｌ２Ｏ３−ＭｇＯ、ＳｉＣ、ＳｉＣ−ＳｉＯ２等が使用される。なかでもＳｉＣは、上記温度域での機械的強度、耐クリープ性、耐熱衝撃性が優れており、より肉薄にできるため省エネ、省スペースが可能であり、またより長期間使用しても損傷が少ない。 As the baking container, Al 2 O 3 , Al 2 O 3 —SiO 2 , Al 2 O 3 .SiO 2 .MgO, Al 2 O 3 —MgO, SiC, SiC—SiO 2 or the like is used. Among these, SiC has excellent mechanical strength, creep resistance, and thermal shock resistance in the above temperature range, and can be made thinner to save energy and save space. Few.
ただし、ＳｉＣの表面に直接、被焼成物を載置すると反応する場合が多く、ＳｉＣを使用するためには、Ａｌ２Ｏ３、ＺｒＯ２等の難反応性の表面被覆が必要である。表面皮膜を形成するためには、基材との密着性を上げるために基材表面を（１）粗面化する、（２）ポーラス（多孔質）な基材を使用する必要がある。 However, in many cases, reaction occurs when an object to be fired is placed directly on the surface of SiC, and in order to use SiC, it is necessary to provide a surface coating with a low reactivity such as Al 2 O 3 or ZrO 2 . In order to form a surface film, it is necessary to (1) roughen the surface of the base material and (2) a porous (porous) base material in order to improve adhesion to the base material.
高温で被焼成物を積載して使用すると、酸化や皮膜に浸透してきた被焼成物成分との反応により基材は劣化する。特に最初に外来成分の影響受ける基材表面部の劣化の度合いは大きい。このため基材を再利用するために皮膜を除去する際に皮膜と一緒に基材表面の凸部がなくなってしまい皮膜を形成するに十分な表面粗さが得られないことが多い。 When a material to be fired is loaded and used at a high temperature, the base material deteriorates due to oxidation or reaction with the material to be fired that has penetrated into the film. In particular, the degree of deterioration of the surface portion of the base material that is initially affected by the foreign component is large. For this reason, when removing a film in order to reuse the base material, the convex portions on the surface of the base material are lost together with the film, and the surface roughness sufficient to form the film is often not obtained.
従って緻密なＳｉＣ質基材ではケミカルエッチングのような再度粗面化処理が必要になる。 Therefore, a rough SiC substrate such as chemical etching is required for a dense SiC substrate.
これに対して、本再生方法の対象になる焼成用容器のポーラス基材では、基材表面部の一部が脆化により欠損したとしても、もともと多数の空孔を持つ組織を有するため、皮膜との密着性のよい表面が常に得られる。従って、本再生方法は再度粗面化を必要とせず、粗面化処理にケミカルエッチングを必要とする緻密質ＳｉＣ質基材を用いる場合に比べて安価に再生ができる。 In contrast, in the porous base material of the firing container that is the subject of this regeneration method, even if a part of the surface portion of the base material is lost due to embrittlement, it originally has a structure with a large number of pores, A surface with good adhesiveness can always be obtained. Therefore, this regeneration method does not require roughening again, and can be regenerated at a lower cost than when using a dense SiC substrate that requires chemical etching for the roughening treatment.
反応性の高い被焼成物を積載する用途で使用された基材で、表面が反応により脆化した場合は脆化部分を研削等の機械的加工で除去した後再利用することもポーラス基材であれば可能である。 Porous base material that is used for loading highly baked objects, and when the surface becomes brittle due to reaction, the brittle part can be removed by mechanical processing such as grinding and reused. If possible.
皮膜との密着性を考慮した場合、見かけ気孔率は１５％以上が必要である。図１及び図２に、見掛け気孔率２７％の多孔質ＳｉＣ質基材に皮膜を形成した断面組織を示す。基材の気孔に皮膜が食い込みアンカー構造を有していることがわかる。 In consideration of adhesion to the film, the apparent porosity needs to be 15% or more. 1 and 2 show a cross-sectional structure in which a film is formed on a porous SiC substrate having an apparent porosity of 27%. It can be seen that the coating bites into the pores of the substrate and has an anchor structure.
見かけ気孔率が１５％未満であると、皮膜と基材間で十分なアンカー効果が得られず、使用初期で剥離が発生する場合がある。 If the apparent porosity is less than 15%, a sufficient anchor effect cannot be obtained between the coating and the substrate, and peeling may occur in the initial stage of use.
見掛け気孔率が増加するほど皮膜の密着性は向上するが、基材の強度が低下する。 As the apparent porosity increases, the adhesion of the film improves, but the strength of the substrate decreases.
強度としては、曲げ強さで３５ＭＰａ以上が必要である。曲げ強さで３５ＭＰａ未満であると、焼成用容器の形状によっては、例えば厚さ１〜３ｍｍの肉薄セッターなどで割れが発生する場合がある。 As the strength, a bending strength of 35 MPa or more is necessary. If the bending strength is less than 35 MPa, cracks may occur, for example, in a thin setter having a thickness of 1 to 3 mm depending on the shape of the baking container.
ポーラス化する手段としては、原料の粒度構成により調整する方法、焼成時に消失する空間形成材の添加、スラリーに気泡を形成した状態で成形する等の方法が挙げられる。焼成は、通常の焼結、反応焼結等いずれの方法でも可能であるが、焼結による収縮を伴わず焼結前の気孔率をほぼ維持できる再結晶による焼結が好ましい。再結晶を進めるには通常１５００〜２５００℃程度の温度での焼結が必要である。 Examples of the porous means include a method of adjusting according to the particle size configuration of the raw material, a method of adding a space forming material that disappears during firing, and a method of forming in a state where bubbles are formed in the slurry. Firing can be performed by any method such as ordinary sintering and reaction sintering, but sintering by recrystallization that can substantially maintain the porosity before sintering without shrinkage due to sintering is preferable. In order to proceed with recrystallization, sintering at a temperature of about 1500 to 2500 ° C. is usually required.
高温（１３００℃以上程度）で、酸素が含まれる雰囲気で使用されると、使用初期にＳｉＣの酸化に伴うガスのやりとりが起こり被焼成物に悪影響を及ぼす場合がある。このような場合は、基材表面に皮膜をつける前に予め酸化した後、皮膜を形成することで初期の酸化に伴う反応の影響を軽減できる。 When used in an atmosphere containing oxygen at a high temperature (about 1300 ° C. or higher), gas exchange accompanying the oxidation of SiC may occur in the initial stage of use, which may adversely affect the material to be fired. In such a case, the effect of the reaction accompanying the initial oxidation can be reduced by forming a film after previously oxidizing the film on the surface of the substrate.
最表面の皮膜としてはチタン酸バリウム、フェライトなどのセラミック電子部品材料と難反応性であるＺｒＯ２やＡｌ２Ｏ３が好ましい。特に多くの材質と難反応性であるＺｒＯ２が好ましい。ＺｒＯ２は基材のＳｉＣに比較して熱膨張が大きいため、高温での使用時には、熱膨張差に起因する応力がＺｒＯ２とＳｉＣ質基材間に発生する。 As the outermost film, ZrO 2 or Al 2 O 3 which is hardly reactive with ceramic electronic component materials such as barium titanate and ferrite is preferable. In particular, ZrO 2 which is hardly reactive with many materials is preferable. Since ZrO 2 has a larger thermal expansion than SiC of the base material, stress due to the thermal expansion difference is generated between the ZrO 2 and the SiC base material when used at a high temperature.
この応力を緩和するために、ＺｒＯ２皮膜とＳｉＣ質基材間に中間の熱膨張を持つＡｌ２Ｏ３、ムライト、ジルコン皮膜を形成すると剥離が起こりにくくなる。 In order to relieve this stress, if an Al 2 O 3 , mullite, or zircon film having an intermediate thermal expansion is formed between the ZrO 2 film and the SiC base material, peeling is less likely to occur.
皮膜の厚さとしては、３０〜５００μｍが好ましい。皮膜の厚さは膜の気孔率、粒の大きさ等で左右されるが３０μｍより薄いと緻密な膜でも部分的に気孔やひびが連鎖し、短時間で基材表面のＳｉＯ２や被焼成物成分が皮膜を通過して、反応が起こり好ましくない。 The thickness of the film is preferably 30 to 500 μm. The thickness of the film depends on the porosity and grain size of the film, but if it is thinner than 30 μm, pores and cracks are partially linked even in a dense film, and the SiO 2 on the substrate surface or fired in a short time. A physical component passes through the film and reacts, which is not preferable.
膜厚が厚くなると皮膜のＳｉＯ２や被焼成物成分が横断するのに要する時間は長くなるが１０００μｍより厚いと、ＳｉＣ質基材と皮膜の熱膨張差により発生する応力の割合が大きくなり剥離が発生しやすくなる。 When the film thickness is increased, the time required for the SiO 2 and the component to be baked to traverse the film becomes longer, but when it is thicker than 1000 μm, the rate of stress generated due to the difference in thermal expansion between the SiC substrate and the film increases and peeling occurs. Is likely to occur.
皮膜の形成にはプラズマ溶射、スラリー塗布焼付け、エアロゾルデポジション、ガスデポジション、ＣＶＤ等の方法がある。 For forming the coating, there are methods such as plasma spraying, slurry coating and baking, aerosol deposition, gas deposition, and CVD.
特に溶融した原料が高速で基材に衝突し瞬時に固化するプラズマ溶射は、ポーラス基材の気孔部に皮膜が食い込み、剥離に対して効果的なアンカー構造を有する皮膜を形成できる。 In particular, plasma spraying in which a molten raw material collides with a base material at high speed and solidifies instantaneously can form a film having an anchor structure effective against peeling by the film biting into the pores of the porous base material.
チタン酸バリウムやフェライト等のセラミック電子部品を積載し、焼成に多数回使用し、皮膜が剥離したり、皮膜表面の反応成分が増加し被積載物との反応が起こり使用できなくなった場合でも、ＳｉＣ質基材自体には割れや反りがないときは、旧皮膜を除去し、新たに皮膜を形成すれば基材を再利用することができる。 Even if ceramic electronic parts such as barium titanate and ferrite are loaded and used many times for firing, the film peels off, or the reaction component on the surface of the film increases and reacts with the load, making it unusable. When the SiC base material itself has no cracks or warpage, the base material can be reused by removing the old film and forming a new film.
皮膜の除去は、ショットブラスト、平面研削等の加工方法を用いることができる。ポーラス基材なので、加工面は適度な空孔を有し皮膜との間にアンカー効果を生む皮膜形成に適した面が得られる。 For removal of the film, a processing method such as shot blasting or surface grinding can be used. Since it is a porous substrate, the processed surface has appropriate pores and a surface suitable for film formation that produces an anchor effect with the film.
必要に応じて再度酸化処理を施した後、初回に皮膜を形成した方法と同様の方法で皮膜を形成する。以上の操作を繰り返すことで多数回の再利用が可能である。 After performing oxidation treatment again if necessary, a film is formed by the same method as that for forming the film for the first time. By repeating the above operation, it can be reused many times.
なお、見かけ気孔率の測定方法及び条件は、ＪＩＳ Ｒ ２２０５「耐火れんがの見掛け気孔率の測定方法」に準じる。曲げ強度の測定方法及び条件は、ＪＩＳ Ｒ ２２１３「耐火れんがの曲げ強さの測定方法」に準じる。プラズマ溶射は水プラズマ溶射であることが好ましい。 The method and conditions for measuring the apparent porosity are in accordance with JIS R 2205 “Method for measuring the apparent porosity of refractory bricks”. The measuring method and conditions of the bending strength are in accordance with JIS R 2213 “Measurement method of bending strength of refractory brick”. The plasma spraying is preferably water plasma spraying.
本実施形態の焼成用容器の再生方法によれば、多孔質ＳｉＣ質基材を用いた焼成用容器の再生に適し、安価な焼成用容器の再生方法が実現する。 According to the firing container regeneration method of the present embodiment, an inexpensive firing container regeneration method is realized that is suitable for regeneration of a firing container using a porous SiC substrate.
（実施例１）
見掛け気孔率２７％の再結晶多孔質ＳｉＣ質基材に水プラズマ溶射法によりアルミナ１５０μｍの皮膜を形成した後、その上に１５０μｍのＺｒＯ２皮膜を形成した。この焼成用容器にチタン酸バリウムを積載して１３５０℃で加熱した。６０時間でいったん温度を下げ皮膜の状態を観察した。この操作を皮膜が剥離するまで繰り返した。延べ１８０時間で部分的に剥離が発生したので、平面研削機を用いて旧皮膜を除去し、最初に皮膜を形成した方法と同様の方法で新たに皮膜を形成した。
Example 1
A 150 μm alumina film was formed on a recrystallized porous SiC substrate having an apparent porosity of 27% by water plasma spraying, and then a 150 μm ZrO 2 film was formed thereon. This firing container was loaded with barium titanate and heated at 1350 ° C. The temperature was lowered once in 60 hours and the state of the film was observed. This operation was repeated until the film peeled off. Since partial peeling occurred in a total of 180 hours, the old film was removed using a surface grinder, and a new film was formed by the same method as the method for forming the film first.
再度同様の加熱試験を行ったところ、２４０時間の時点で剥離が認められ、初回の皮膜と同等以上の皮膜の耐久性が確認された。 When the same heating test was performed again, peeling was observed at 240 hours, and the durability of the film equal to or higher than that of the first film was confirmed.
（比較例１）
見掛け気孔率０％の常圧焼結ＳｉＣ質基材の表面をケミカルエッチングして粗面化した後、実施例１と同様の水プラズマ溶射法によりアルミナ１５０μｍの皮膜を形成した後、その上に１５０μｍのＺｒＯ２皮膜を形成した。実施例１と同様の加熱試験を行ったところ１２０時間で剥離が発生した。基材には割れ、反り等の損傷がなかったので再利用を試みた。
(Comparative Example 1)
After the surface of an atmospheric pressure sintered SiC substrate having an apparent porosity of 0% is chemically etched and roughened, a film of 150 μm alumina is formed by the same water plasma spraying method as in Example 1, and then on the surface. A 150 μm ZrO 2 film was formed. When the same heating test as in Example 1 was performed, peeling occurred in 120 hours. Since the base material was not damaged such as cracking or warping, it was tried to reuse.
平面研削機を用いて旧皮膜を除去し、最初に皮膜を形成した方法と同様の方法で新たな皮膜の形成を試みたが基材の表面粗さが不十分なため皮膜を形成することができなかった。 The old film was removed using a surface grinder, and a new film was formed using the same method as that used to form the film, but the film could be formed because the surface roughness of the substrate was insufficient. could not.
Claims (5)
見かけ気孔率が１５％以上であり、
かつ、曲げ強さが３５ＭＰａ以上である多孔質ＳｉＣ質基材の少なくとも前記被焼成物を載置する部分の表面に、
Ａｌ２Ｏ３、ＺｒＯ２、ムライト（Ａｌ２Ｏ３−ＳｉＯ２）、ジルコン（ＺｒＳｉＯ４）の少なくとも１種または複数を主成分とするセラミックス皮膜を形成した焼成用容器を、
数回使用した後に、前記多孔質ＳｉＣ質基材の前記表面に形成されていた前記セラミックス皮膜を除去し、
新たにＡｌ２Ｏ３、ＺｒＯ２、ムライト、ジルコンの少なくとも１種または複数を主成分とするセラミックス皮膜を厚さ３０〜５００μｍ形成し、
再生することを特徴とする焼成用容器の再生方法。 Place and use ceramic parts to be fired,
The apparent porosity is 15% or more,
And at least on the surface of the portion on which the object to be fired is placed of the porous SiC base material having a bending strength of 35 MPa or more,
A firing container in which a ceramic film mainly composed of at least one of Al 2 O 3 , ZrO 2 , mullite (Al 2 O 3 —SiO 2 ), and zircon (ZrSiO 4 ) is formed,
After using several times, the ceramic film formed on the surface of the porous SiC substrate is removed,
A ceramic film mainly having at least one or more of Al 2 O 3 , ZrO 2 , mullite, and zircon as a main component is formed to a thickness of 30 to 500 μm,
A method for regenerating a firing container, characterized by regenerating.
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| TW97124390A TWI383965B (en) | 2007-06-28 | 2008-06-27 | A ceramic material for a ceramic ceramic container, a method for manufacturing the same, and a method for producing the same |
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