JPH10272614A - Manufacture of bonded sintered product of high-purity ceramics - Google Patents

Manufacture of bonded sintered product of high-purity ceramics

Info

Publication number
JPH10272614A
JPH10272614A JP7927297A JP7927297A JPH10272614A JP H10272614 A JPH10272614 A JP H10272614A JP 7927297 A JP7927297 A JP 7927297A JP 7927297 A JP7927297 A JP 7927297A JP H10272614 A JPH10272614 A JP H10272614A
Authority
JP
Japan
Prior art keywords
adhesive layer
ceramic
bonded
purity
molding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP7927297A
Other languages
Japanese (ja)
Inventor
Hajime Tanabe
元 田辺
Noritatsu Sawada
昇龍 沢田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JGC Corp
Original Assignee
JGC Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JGC Corp filed Critical JGC Corp
Priority to JP7927297A priority Critical patent/JPH10272614A/en
Publication of JPH10272614A publication Critical patent/JPH10272614A/en
Pending legal-status Critical Current

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  • Laminated Bodies (AREA)
  • Ceramic Products (AREA)
  • Devices For Post-Treatments, Processing, Supply, Discharge, And Other Processes (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a method for manufacturing a bonded sintered product of high-purity ceramics by which it is possible to obtain an integrated sintered product of bonded ceramics by sinter-bonding unsintered high-purity ceramic moldings. SOLUTION: This method for manufacturing a bonded sintered product of high-purity ceramics comprises a molding step for molding a molding material containing high-purity ceramic powder and an organic binder, an adhesive layer forming step for forming an adhesive layer containing, preferably an identical organic binder to the organic binder contained in the molding material, on the surface of ceramic moldings obtained in the molding step, a laminating step for laminating other ceramic moldings to the ceramic moldings with the adhesive layer, and a sintering step for sintering the laminated moldings. Through the sintering step, the moldings are effectively bonded to each other to obtain a bonded sintered product. The thickness of the adhesive layer is preferably within the range of 0.5-20 μm, and the high level of bonding is obtained by adding ceramic powder to the adhesive layer.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、高純度セラミック
の接合焼結方法に関し、特に窪みつき高純度セラミック
基板の製造に好適である高純度セラミック接合焼結体の
製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for bonding and sintering high-purity ceramics, and more particularly to a method for manufacturing a high-purity ceramic bonded sintered body suitable for manufacturing a recessed high-purity ceramic substrate.

【0002】[0002]

【従来の技術】未焼結のセラミック成形体同士を接合し
て、これを焼結して一体化させたセラミック接合焼結体
は、ガラス材あるいはガラスを添加したセラミック成形
体を重ね合わせ焼成することによって容易に得ることが
できる。この容易さは、主成分がガラスまたはガラス成
分を比較的多く含んでいるセラミック粉末からなる成形
体同士を単に重ね合わせた状態で焼成したとき、成形体
同士が接している面においてガラスが溶融し結合を生じ
せしめることによるものである。一方、同様にしてガラ
スを含まない高純度セラミック成形体同士を重ね合わせ
た状態で焼成しても、ガラスを含んでいないため成形体
が接している面は一体化せずに接合されない。このよう
に、高純度セラミックの接合焼結体の製造は従来困難で
あった。
2. Description of the Related Art Unsintered ceramic compacts are joined together, sintered and integrated into a ceramic joined sintered compact, and a glass compact or a ceramic compact containing glass is added and fired. Can easily be obtained. This ease is due to the fact that when the compacts made of glass or ceramic powder containing a relatively large amount of glass components are fired in a state in which the compacts are simply overlapped, the glass melts on the surface where the compacts are in contact with each other. This is due to the formation of a bond. On the other hand, even if the high-purity ceramic molded bodies containing no glass are fired in a stacked state in the same manner, the surfaces in contact with the molded bodies are not joined without being integrated because they do not contain glass. As described above, it has been conventionally difficult to manufacture a bonded sintered body of a high-purity ceramic.

【0003】[0003]

【発明が解決しようとする課題】本発明は、上述のごと
き実情に鑑みてなされたもので、未焼結の高純度セラミ
ック成形体同士を焼結により接合し、一体となったセラ
ミック接合焼結体を得るための高純度セラミックの接合
焼結体の製造方法を提供することをその解決すべき課題
とする。
SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned circumstances, and combines unsintered high-purity ceramic compacts by sintering to form an integrated ceramic joint sintered body. It is an object of the present invention to provide a method for producing a bonded sintered body of a high-purity ceramic for obtaining a body.

【0004】[0004]

【課題を解決するための手段】請求項1の発明は、高純
度セラミック粉末と成形用有機バインダとを含んでなる
セラミック成形材料を成形し、セラミック成形体を得る
成形工程と、該成形工程で得られる前記セラミック成形
体の表面に接着層用有機バインダを含んでなる接着層を
形成する接着層形成工程と、前記接着層を形成した前記
セラミック成形体に、前記接着層を介して前記セラミッ
ク成形体を貼り合わせて、貼り合わせ成形体を得る貼り
合わせ工程と、該貼り合わせ成形体を焼結する焼結工程
とを有することを特徴とし、ガラスを含まない高純度セ
ラミックであっても、有機バインダによる接着層を用い
ることにより、接合部の剥離や一部の未接合部を生じさ
せることなく良好に一体化した接合焼結体を得ることが
でき、従来複雑な加工が必要であった構造を有するセラ
ミック焼結体を、焼結前に単純な加工を施した成形体を
貼り合わせてこれを焼結することにより容易に得ること
ができるようにしたものである。
According to the first aspect of the present invention, there is provided a molding step of molding a ceramic molding material containing a high-purity ceramic powder and an organic binder for molding to obtain a ceramic molded body. An adhesive layer forming step of forming an adhesive layer containing an organic binder for an adhesive layer on the surface of the obtained ceramic molded body; and forming the ceramic molded body through the adhesive layer on the ceramic molded body having the adhesive layer formed thereon. It is characterized by having a laminating step of laminating a body to obtain a laminated molded body, and a sintering step of sintering the laminated molded body. By using an adhesive layer made of a binder, it is possible to obtain a well-integrated bonded sintered body without causing peeling of a bonded portion or partial unbonded portion. A ceramic sintered body having a structure that required a work, which can be easily obtained by pasting a molded body which has been subjected to simple processing before sintering and sintering it. .

【0005】請求項2の発明は、請求項1の発明におい
て、前記貼り合わせ工程を経た前記接着層の厚みが0.
5〜20μmの範囲となるようにしたことを特徴とし、
良好な接合部を有する接合焼結体を得るための接着層厚
みのより具体的な範囲が与えられるようにしたものであ
る。
According to a second aspect of the present invention, in the first aspect of the present invention, the thickness of the adhesive layer after the laminating step is set to be 0.5.
Characterized in that it is in the range of 5 to 20 μm,
A more specific range of the thickness of the adhesive layer for obtaining a bonded sintered body having a good bonded portion is provided.

【0006】請求項3の発明は、請求項1または2の発
明において、前記成形用有機バインダ及び前記接着層用
有機バインダとして互いに同一の有機バインダを用いる
ようにしたことを特徴とし、接合部の一体化をより効率
的にかつ確実になすことができるようにしたものであ
る。
According to a third aspect of the present invention, in the first or second aspect of the present invention, the same organic binder is used as the organic binder for molding and the organic binder for the adhesive layer. The integration can be performed more efficiently and reliably.

【0007】請求項4の発明は、請求項1ないし3のい
ずれかの発明において、前記接着層形成工程は、前記セ
ラミック成形材料の組成の少なくとも一部に一致する組
成を有する材料を前記接着層に添加するようにしたこと
を特徴とし、接合部の一体化をより効率的にかつ確実に
なすことができるようにしたものである。
According to a fourth aspect of the present invention, in the first aspect of the present invention, in the bonding layer forming step, a material having a composition corresponding to at least a part of the composition of the ceramic molding material is used. In addition, it is characterized in that the joining portion can be more efficiently and reliably integrated.

【0008】[0008]

【発明の実施の形態】本発明の高純度セラミック接合焼
結体の製造方法おいては以下の工程が必要である。 高純度セラミック粉末からなる未焼結の成形体表面
に、有機バインダ(好ましくは成形体に含有される有機
バインダと同一の有機バインダ)を含む接着層を形成す
る。この接着層は成形体同士を貼り合わせた面すなわち
焼結体接合面の一体化に寄与する。この接着層が無い場
合、貼り合わせた面が焼成中に剥離してしまったり、焼
結体としての接合面に欠陥が生じたりしてしまう。 上記の接着層を形成した面で接合すべき未焼結の成形
体同士を貼り合わせる。この工程は未焼結の高純度セラ
ミック成形体を形成するものである。例えば、所定の孔
加工を施したグリーンシートを貼り合わせることにより
窪みのついた基板用の成形体を容易に形成することがで
きる。 貼り合わせた成形体を所望の密度が得られるように焼
結する。 以上の工程によって高純度セラミック接合焼結体を得る
ことができる。
BEST MODE FOR CARRYING OUT THE INVENTION The following steps are required in the method for producing a high-purity ceramic bonded sintered body of the present invention. An adhesive layer containing an organic binder (preferably the same organic binder as the organic binder contained in the molded body) is formed on the surface of the unsintered molded body made of the high-purity ceramic powder. This adhesive layer contributes to the integration of the surface where the molded bodies are bonded to each other, that is, the bonding surface of the sintered body. If the adhesive layer is not provided, the bonded surfaces may be peeled off during firing, or defects may occur on the bonding surface as a sintered body. The unsintered compacts to be joined on the surface on which the adhesive layer is formed are attached to each other. This step forms an unsintered high-purity ceramic compact. For example, a green body for a substrate having a depression can be easily formed by bonding green sheets having been subjected to predetermined hole processing. The bonded compact is sintered so as to obtain a desired density. Through the above steps, a high-purity ceramic bonded sintered body can be obtained.

【0009】本発明の未焼結の高純度セラミック成形体
は99%以上の純度を持つガラス以外のもので、セラミ
ックの焼結に必要な助材や安定化剤などが含まれていて
もよい。例えば、好適な材料としては99.9%Al2
3,やY23,MgO,CaO,CeO2などの安定化剤
を添加したZrO2などが挙げられる。
The non-sintered high-purity ceramic compact of the present invention is other than glass having a purity of 99% or more, and may contain auxiliary materials and stabilizers necessary for sintering the ceramic. . For example, a preferred material is 99.9% Al 2 O
And ZrO 2 to which a stabilizer such as Y 2 O 3 , MgO, CaO, or CeO 2 is added.

【0010】貼り合わせる高純度セラミック成形体は乾
式プレス法、ドクターブレード法などの成形方法により
所望の形状が得られた成形体でよく、また成形用バイン
ダの種類にも制限はない。
The high-purity ceramic molded body to be bonded may be a molded body having a desired shape obtained by a molding method such as a dry pressing method or a doctor blade method, and the type of the molding binder is not limited.

【0011】また、成形体表面に塗布する接着層用のバ
インダは有機系バインダを用いるが、このとき貼り合わ
せようとする成形体に含まれている有機バインダと相溶
性があるバインダを選択し、好ましくは焼結の際、脱脂
に支障がない同一系の有機バインダを使用することが望
ましい。また、接合面の一体化を助長する方法として、
例えば成形体と同一のセラミック粉末やセラミック成形
体の焼結助材を接着層用の有機バインダに添加すること
もできる。
An organic binder is used as a binder for the adhesive layer applied to the surface of the molded body. At this time, a binder compatible with the organic binder contained in the molded body to be bonded is selected. It is preferable to use the same organic binder that does not hinder degreasing during sintering. Also, as a method to promote the integration of the joining surface,
For example, the same ceramic powder as the compact or a sintering aid for the ceramic compact can be added to the organic binder for the adhesive layer.

【0012】高純度セラミック成形体表面に前記有機バ
インダによる接着剤を塗布しこれを乾燥することにより
形成される接着層の厚みは、0.5〜20μmの範囲で
ある必要がある。接着層の厚みが20μmを超えると貼
り合わせ面の高純度セラミック同士の接触が不十分にな
り一体となって焼結しない。また、0.5μmより薄く
なると均一に接着層を形成することが困難になり、接合
焼結体の接合面に部分的な未接合状態が生じてしまう。
The thickness of the adhesive layer formed by applying the adhesive made of the organic binder to the surface of the high-purity ceramic molded body and drying the applied adhesive must be in the range of 0.5 to 20 μm. If the thickness of the adhesive layer exceeds 20 μm, the high-purity ceramics on the bonding surface will not be in sufficient contact with each other and will not be sintered together. On the other hand, when the thickness is less than 0.5 μm, it is difficult to form an adhesive layer uniformly, and a partial unbonded state occurs on the bonded surface of the bonded sintered body.

【0013】高純度セラミック成形体の接合したい面に
接着層用の有機バインダを塗布しこれを乾燥後、貼り合
わせた面に間隙が残存しないようプレス機を使用する。
ここで、加熱しながら貼り合わせると接合面の一体化に
効果がある。また、塗布したバインダが乾燥したときに
貼り合わせ面に気泡などが生じなければ塗布したバイン
ダの乾燥前に成形体を貼り合わせてもよい。
An organic binder for an adhesive layer is applied to the surface of the high-purity ceramic molded body to be joined and dried, and then a pressing machine is used so that no gap remains on the bonded surface.
Here, bonding while heating is effective in integrating the bonding surfaces. Further, if air bubbles or the like are not generated on the bonding surface when the applied binder is dried, the molded body may be bonded before the applied binder is dried.

【0014】貼り合わせた成形体は、所望の密度が得ら
れるよう焼結することにより高純度セラミック接合焼結
体を得ることができる。
The bonded compact is sintered so as to obtain a desired density, whereby a high-purity ceramic bonded sintered body can be obtained.

【0015】以下に本発明による高純度セラミック接合
焼結体の製造方法による実施例を比較例と共により具体
的に説明する。高純度アルミナ(99.9%)粉末、P
VB(ポリビニルブチラール)、トリオレイングリコー
ル、ジブチルフタレート、及びエチルアルコールをボー
ルミルで分散混合し、ドクターブレードを用いて0.2
mmの厚みをもったグリーンシートを作製した。このグ
リーンシートの表面に、PVBをエチルアルコールで溶
かしたバインダをスクリーン印刷機で均一に塗布した。
このときの塗布厚は後述する乾燥工程により得られる接
着層としての層厚が0.5〜20μmの範囲となるよう
に設定した。塗布したバインダを90℃で10分間乾燥
させた後、接着層を挟むようにして2枚のグリーシート
同士を重ね合わせ100℃に加熱しながら加圧した。こ
の貼り合わせたグリーンシートを大気中で焼結し、高純
度アルミナ接合焼結体を得た。同様にして3mol%Y
23を添加したZrO2の接合焼結体も作製した。得ら
れたそれぞれの接合焼結体を破断し、接合部分の破断面
をSEMによって観察した。この結果を表1に示す。表
1では接合面の評価が良好なものは○で、接合面に不具
合の生じたものを×で表わしている。
Examples of the method for manufacturing a high-purity ceramic bonded sintered body according to the present invention will be described below in more detail with reference to comparative examples. High purity alumina (99.9%) powder, P
VB (polyvinyl butyral), triolein glycol, dibutyl phthalate, and ethyl alcohol are dispersed and mixed by a ball mill, and 0.2 is mixed with a doctor blade.
A green sheet having a thickness of mm was produced. A binder obtained by dissolving PVB with ethyl alcohol was uniformly applied to the surface of the green sheet using a screen printer.
The coating thickness at this time was set such that the layer thickness as an adhesive layer obtained by a drying step described later was in the range of 0.5 to 20 μm. After the applied binder was dried at 90 ° C. for 10 minutes, two grease sheets were overlapped with each other so as to sandwich the adhesive layer, and pressurized while heating to 100 ° C. The bonded green sheets were sintered in the air to obtain a high-purity alumina bonded sintered body. Similarly, 3 mol% Y
A bonded sintered body of ZrO 2 to which 2 O 3 was added was also prepared. Each of the obtained bonded sintered bodies was fractured, and the fracture surface of the bonded portion was observed by SEM. Table 1 shows the results. In Table 1, those with good evaluation of the bonding surface are represented by ○, and those having a failure on the bonding surface are represented by x.

【0016】[0016]

【表1】 [Table 1]

【0017】表1に示すごとくに接着層の厚みが0.5
〜10μmのとき、接合部は良好に接合された。接着層
の厚みが0μmのものと20μmを越えるものについて
は、接合部に一部の未接合が生じるかまたは全く接合せ
ずに剥離してしまった。
As shown in Table 1, the thickness of the adhesive layer was 0.5
When the thickness was 10 μm to 10 μm, the joint was satisfactorily joined. When the thickness of the adhesive layer was 0 μm or more than 20 μm, some unbonded portions were formed at the bonded portions, or they were separated without bonding at all.

【0018】[0018]

【発明の効果】【The invention's effect】

請求項1の効果:ガラスを含まない高純度セラミックで
あっても、有機バインダによる接着層を用いることによ
り、接合部の剥離や一部の未接合部を生じさせることな
く良好に一体化した接合焼結体を得ることができ、従来
複雑な加工が必要であった構造を有するセラミック焼結
体を、焼結前に単純な加工を施した成形体を貼り合わせ
てこれを焼結することにより容易に得ることができる。
Advantageous Effect of Claim 1: Even in the case of high-purity ceramics not containing glass, by using an adhesive layer made of an organic binder, bonding is successfully integrated without causing peeling of a bonded portion or partial unbonded portion. A sintered body can be obtained, and a ceramic sintered body having a structure that conventionally required complicated processing is bonded to a molded body that has been subjected to simple processing before sintering and sintered. Can be easily obtained.

【0019】請求項2の効果:良好な接合部を有する接
合焼結体を得るための接着層厚みのより具体的な範囲が
与えられる。
Effect of Claim 2: A more specific range of the adhesive layer thickness for obtaining a bonded sintered body having a good bonded portion is provided.

【0020】請求項3の効果:成形体に含まれる有機バ
インダと接着材料層に含まれる有機バインダとを互いに
同一の有機バインダとすることにより、接合部の一体化
をより効率的かつ確実になすことができる。
According to the third aspect of the present invention, the organic binder contained in the molded article and the organic binder contained in the adhesive material layer are the same organic binder, so that the joint can be more efficiently and reliably integrated. be able to.

【0021】請求項4の効果:成形体の主成分であるセ
ラミック粉末等の成形体に含まれる組成を有する材料を
接着層に添加することにより、接合部の一体化をより効
率的かつ確実になすことができる。
According to the fourth aspect, by adding a material having a composition contained in the molded body, such as ceramic powder, which is a main component of the molded body, to the adhesive layer, the joining portion can be more efficiently and reliably integrated. I can do it.

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 高純度セラミック粉末と成形用有機バイ
ンダとを含んでなるセラミック成形材料を成形し、セラ
ミック成形体を得る成形工程と、該成形工程で得られる
前記セラミック成形体の表面に接着層用有機バインダを
含んでなる接着層を形成する接着層形成工程と、前記接
着層を形成した前記セラミック成形体に、前記接着層を
介して前記セラミック成形体を貼り合わせて、貼り合わ
せ成形体を得る貼り合わせ工程と、該貼り合わせ成形体
を焼結する焼結工程とを有することを特徴とする高純度
セラミック接合焼結体の製造方法。
1. A molding step of molding a ceramic molding material containing high-purity ceramic powder and an organic binder for molding to obtain a ceramic molding, and an adhesive layer on a surface of the ceramic molding obtained in the molding step. An adhesive layer forming step of forming an adhesive layer containing an organic binder for use, and bonding the ceramic molded body via the adhesive layer to the ceramic molded body on which the adhesive layer has been formed, thereby forming a bonded molded body. A method for producing a high-purity ceramic bonded sintered body, comprising: a bonding step for obtaining; and a sintering step for sintering the bonded molded body.
【請求項2】 前記貼り合わせ工程を経た前記接着層の
厚みが0.5〜20μmの範囲となるようにしたことを
特徴とする請求項1に記載の高純度セラミック接合焼結
体の製造方法。
2. The method for manufacturing a high-purity ceramic bonded sintered body according to claim 1, wherein the thickness of the adhesive layer after the bonding step is in a range of 0.5 to 20 μm. .
【請求項3】 前記成形用有機バインダ及び前記接着層
用有機バインダとして互いに同一の有機バインダを用い
るようにしたことを特徴とする請求項1または2に記載
の高純度セラミック接合焼結体の製造方法。
3. The high-purity ceramic bonded sintered body according to claim 1, wherein the same organic binder is used as the organic binder for molding and the organic binder for the adhesive layer. Method.
【請求項4】 前記接着層形成工程は、前記セラミック
成形材料の組成の少なくとも一部に一致する組成を有す
る材料を前記接着層に添加するようにしたことを特徴と
する請求項1ないし3のいずれか1に記載の高純度セラ
ミック接合焼結体の製造方法。
4. The adhesive layer forming step according to claim 1, wherein a material having a composition corresponding to at least a part of the composition of the ceramic molding material is added to the adhesive layer. The method for producing a high-purity ceramic bonded sintered body according to any one of the first to third aspects.
JP7927297A 1997-03-31 1997-03-31 Manufacture of bonded sintered product of high-purity ceramics Pending JPH10272614A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7927297A JPH10272614A (en) 1997-03-31 1997-03-31 Manufacture of bonded sintered product of high-purity ceramics

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7927297A JPH10272614A (en) 1997-03-31 1997-03-31 Manufacture of bonded sintered product of high-purity ceramics

Publications (1)

Publication Number Publication Date
JPH10272614A true JPH10272614A (en) 1998-10-13

Family

ID=13685237

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7927297A Pending JPH10272614A (en) 1997-03-31 1997-03-31 Manufacture of bonded sintered product of high-purity ceramics

Country Status (1)

Country Link
JP (1) JPH10272614A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005508723A (en) * 2001-03-08 2005-04-07 ザ・リージェンツ・オブ・ジ・ユニバーシティ・オブ・カリフォルニア Method for manufacturing thick film and / or thin film

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005508723A (en) * 2001-03-08 2005-04-07 ザ・リージェンツ・オブ・ジ・ユニバーシティ・オブ・カリフォルニア Method for manufacturing thick film and / or thin film

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