JP2015048272A - Ceramic sintered body and manufacturing method thereof - Google Patents
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- 239000000919 ceramic Substances 0.000 title claims abstract description 107
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims description 37
- 238000005304 joining Methods 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 7
- 230000006866 deterioration Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- 239000002245 particle Substances 0.000 description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 15
- 239000002994 raw material Substances 0.000 description 14
- 239000011230 binding agent Substances 0.000 description 12
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000005452 bending Methods 0.000 description 6
- 238000010304 firing Methods 0.000 description 4
- 239000011343 solid material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000007429 general method Methods 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明は、セラミックス焼結体およびその製造方法に関する。 The present invention relates to a ceramic sintered body and a method for producing the same.
未焼結のセラミックス成形体同士を、当該セラミックスと同組成のスラリーを接合材として接合させたうえで焼結して一体化させることによりセラミックス焼結体を製造する方法が提案されている（特許文献１参照）。 There has been proposed a method of manufacturing a ceramic sintered body by bonding unsintered ceramic compacts together with a slurry having the same composition as the ceramic as a bonding material and then sintering and integrating them (patent) Reference 1).
しかし、当該手法によれば、焼結体においてもとは成形体同士の接合界面であった箇所に隙間が存在するため、当該箇所の強度が局所的に低下する。 However, according to the method, since there is a gap at a place where the sintered body was originally a bonding interface between the molded bodies, the strength of the place is locally reduced.
そこで、本発明は、セラミックス成形体同士が接合されたことに由来する強度低下の低減が図られているセラミックス焼結体およびその製造方法を提供することを目的とする。 Then, an object of this invention is to provide the ceramic sintered compact by which the reduction | decrease of the strength reduction resulting from joining the ceramic molded bodies is aimed at, and its manufacturing method.
本発明は、以下の［１］〜［３］のセラミックス焼結体の製造方法を提供する。
［１］同一組成の複数のセラミックス成形体を準備する工程と、
前記複数のセラミックス成形体のうち少なくとも１つに、前記複数のセラミックス成形体同士の接合領域から当該接合領域の境界まで連続する幅０．０１〜０．５［ｍｍ］かつ当該幅の０．４〜１．０倍の深さの、屈曲箇所が存在しない曲線状の断面形状を有するような溝を形成する工程と、
前記複数のセラミックス成形体と同一組成のセラミックス粉末が分散されているスラリーを前記接合領域に付着させる工程と、
前記複数のセラミックス成形体同士を前記接合領域において接合させる工程と、
当該接合された前記複数のセラミックス成形体を焼結して一体化する工程と、を含むセラミックス焼結体の製造方法。
［２］前記接合領域における面積占有率が０．２〜４５％になるように前記溝が形成される［１］記載の方法。
The present invention provides a method for producing a ceramic sintered body according to the following [1] to [3].
[1] preparing a plurality of ceramic molded bodies having the same composition;
At least one of the plurality of ceramic compacts has a width of 0.01 to 0.5 [mm] continuous from the joint region between the ceramic compacts to the boundary of the joint region, and 0.4 of the width. A step of forming a groove having a curved cross-sectional shape with no bent portion at a depth of -1.0 times;
Attaching a slurry in which ceramic powder having the same composition as the plurality of ceramic molded bodies is dispersed to the joining region;
Bonding the plurality of ceramic molded bodies to each other in the bonding region;
A step of sintering and integrating the plurality of joined ceramic molded bodies.
[2] The method according to [1], wherein the groove is formed so that an area occupation ratio in the bonding region is 0.2 to 45%.
本発明は、以下の［３］のセラミックス焼結体を提供する。
［３］［１］または［２］記載の方法により製造された、外部に連通する内部空間を有するセラミックス焼結体であって、前記内部空間を画定する側壁に前記溝からはみ出した前記スラリーに由来する局所的な凸部が形成されているセラミックス焼結体。
The present invention provides the following ceramic sintered body [3].
[3] A ceramic sintered body having an internal space communicating with the outside, manufactured by the method according to [1] or [2], wherein the slurry protrudes from the groove on a side wall defining the internal space. A ceramic sintered body in which local protrusions are derived.
本発明の方法および当該方法により製造されたセラミックス焼結体によれば、セラミックス成形体同士の接合領域に付着されたスラリーに含まれる気泡を、溝を通じて当該接合領域の内側から外側に逃がすことができる。セラミックス成形体の接合体（接合成形体）が焼成過程において約２０％収縮するが、溝が曲線状の断面形状を有する（屈曲箇所が存在しない）ため、当該屈曲箇所に対する応力の集中によって焼結体にクラックが発生する可能性の低減が図られる。このため、当該気泡に由来する隙間による強度低下度の低減が図られている。 According to the method of the present invention and the ceramic sintered body produced by the method, bubbles contained in the slurry adhered to the joining region between the ceramic molded bodies can be released from the inside to the outside of the joining region through the groove. it can. The ceramic compact joined body (joined compact) shrinks by about 20% during the firing process, but since the groove has a curved cross-sectional shape (there is no bent part), sintering is caused by the concentration of stress on the bent part. The possibility of cracks occurring in the body is reduced. For this reason, reduction of the strength reduction degree by the clearance gap derived from the said bubble is aimed at.
本発明の一実施形態としてのセラミックス焼結体の製造方法は、図１（１）〜（５）に概略的に示されている（１）成形体準備工程と、（２）溝形成工程と、（３）スラリー付着工程と、（４）接合工程と、（５）焼結工程と、を含んでいる。 The method for manufacturing a ceramic sintered body according to an embodiment of the present invention includes (1) a molded body preparing step and (2) a groove forming step schematically shown in FIGS. 1 (1) to (5). , (3) a slurry adhesion step, (4) a joining step, and (5) a sintering step.
（１）成形体準備工程
図（１）に示されているように、複数のセラミックス成形体Ｃ１およびＣ２が準備される。具体的には、アクリルエマルジョン等の適当なバインダが添加されたセラミックス粉末が、ＣＩＰまたは鋳込み等の一般的な手法にしたがって成形されることにより複数の成形体Ｃ１およびＣ２が準備される。複数の成形体Ｃ１およびＣ２が一の成形体から切り出されることにより準備されてもよい。
(1) Molded body preparation step As shown in FIG. (1), a plurality of ceramic molded bodies C1 and C2 are prepared. Specifically, a plurality of molded bodies C1 and C2 are prepared by molding ceramic powder to which an appropriate binder such as acrylic emulsion is added according to a general technique such as CIP or casting. The plurality of molded bodies C1 and C2 may be prepared by being cut out from one molded body.
セラミックス粉末としては、アルミナ、マグネシア、スピネル、ジルコニア、イットリア等の酸化物、炭化珪素等の炭化物、窒化珪素、窒化アルミニウム等の窒化物等種々のセラミックスが適用できる。これらを複数用いた混合物、または必要に応じて焼結助剤等の上記以外の成分を含ませることも可能である。これらは市販のセラミックス粉末を用いることができる。平均粒径０．１〜２．０［μｍ］のセラミックス粉末が原料として用いられることが好ましい。 As the ceramic powder, various ceramics such as oxides such as alumina, magnesia, spinel, zirconia, yttria, carbides such as silicon carbide, nitrides such as silicon nitride and aluminum nitride can be applied. It is also possible to include a mixture using a plurality of these, or, if necessary, other components such as a sintering aid. Commercially available ceramic powder can be used for these. A ceramic powder having an average particle size of 0.1 to 2.0 [μm] is preferably used as a raw material.
（２）溝形成工程
図１（２）に示されているように、複数のセラミックス成形体Ｃ１およびＣ２のうち少なくとも１つ（たとえば成形体Ｃ１）に、当該セラミックス成形体Ｃ１およびＣ２同士の接合領域から当該接合領域の境界まで連続するように溝Ｇが形成される。溝Ｇはフライス盤を用いたフェイスミル加工等の一般的方法により形成されうる。
(2) Groove formation step As shown in FIG. 1 (2), at least one of the plurality of ceramic molded bodies C1 and C2 (for example, the molded body C1) is joined to the ceramic molded bodies C1 and C2. The groove G is formed so as to continue from the region to the boundary of the bonding region. The groove G can be formed by a general method such as face milling using a milling machine.
たとえば、図２（ａ）に示されているように、矩形状のセラミックス成形体Ｃ１の上面（他方のセラミックス成形体Ｃ２との接合領域を構成する）に、上辺の一点と下片の一点とを結ぶように直線状に延在するＮ１本（図２ではＮ１＝３）の縦溝Ｇ１と、左辺の一点と右片の一点とを結ぶように直線状に延在するＮ２本（図２ではＮ２＝３）の横溝Ｇ２とが、溝Ｇとして形成される。図２（ｂ）に示されているように、一方のセラミックス成形体Ｃ１の上面に縦溝Ｇ１が形成され、他方のセラミックス成形体Ｃ２の下面に横溝Ｇ２が形成されてもよい。溝Ｇは直線状ではなく、円弧状または波線状などの曲線状であってもよい。 For example, as shown in FIG. 2 (a), one point on the upper side and one point on the lower piece are formed on the upper surface of the rectangular ceramic molded body C1 (which constitutes a joining region with the other ceramic molded body C2). N1 (N1 = 3 in FIG. 2) longitudinal grooves G1 extending linearly and N2 extending linearly so as to connect one point on the left side and one point on the right piece (FIG. 2). Then, the lateral groove G2 of N2 = 3) is formed as the groove G. As shown in FIG. 2B, the vertical groove G1 may be formed on the upper surface of one ceramic molded body C1, and the horizontal groove G2 may be formed on the lower surface of the other ceramic molded body C2. The groove G is not linear, but may be a curved line such as an arc or a wavy line.
セラミックス成形体Ｃ１の上面およびセラミックス成形体Ｃ２の下面の一方または両方に、製造対象であるセラミックス焼結体ＳＣの内部空間を構成する凹部または溝部が形成されている場合、当該凹部に連続するように溝Ｇが形成されていてもよい。説明の簡単のため、セラミックス成形体Ｃ１およびＣ２の接合領域の境界のうち凹部との境界を「内縁」といい、その他の部分を「外縁」という。 When a concave portion or a groove portion constituting the internal space of the ceramic sintered body SC to be manufactured is formed on one or both of the upper surface of the ceramic molded body C1 and the lower surface of the ceramic molded body C2, it is continuous with the concave portion. A groove G may be formed in the groove. For the sake of simplicity of explanation, the boundary between the ceramic molded bodies C1 and C2 and the recess is referred to as “inner edge” and the other part as “outer edge”.
たとえば、図３（ａ）左側に示されているように一のセラミックス成形体Ｃ１の上面中央に縦に延在する凹部Ｒ１と、当該凹部Ｒ１にのみ連続するように横に延在する溝Ｇ１が形成される。図３（ａ）右側に示されているように他のセラミックス成形体Ｃ２の下面中央に縦に延在する凹部Ｒ２と、凹部Ｒ２から離れて当該下面の境界に連続するように（溝Ｇ１と縦方向について同じ位置で）横に延在する溝Ｇ２が形成される。当該構成のセラミックス成形体Ｃ１およびＣ２が接合されることで、図３（ｂ）に示されているようにセラミックス接合成形体Ｃにおいて凹部Ｒ１およびＲ２により縦に延在する内部空間Ｒ（または通路）が構成され、溝Ｇ１およびＧ２により接合領域（斜線部分）の外縁および内縁（または内部空間Ｒ）に連通する溝Ｇが構成される。 For example, as shown on the left side of FIG. 3A, a concave portion R1 that extends vertically in the center of the upper surface of one ceramic molded body C1, and a groove G1 that extends laterally so as to continue only to the concave portion R1. Is formed. As shown on the right side of FIG. 3 (a), a recess R2 that extends vertically in the center of the lower surface of another ceramic molded body C2, and is separated from the recess R2 and continues to the boundary of the lower surface (groove G1 and A groove G2 is formed which extends laterally (at the same position in the longitudinal direction). By joining the ceramic molded bodies C1 and C2 having the above configuration, as shown in FIG. 3 (b), the internal space R (or the passage) extending vertically by the recesses R1 and R2 in the ceramic bonded molded body C. ) And a groove G communicating with the outer edge and the inner edge (or the inner space R) of the joining region (shaded portion) is formed by the grooves G1 and G2.
溝Ｇの断面形状は、屈曲箇所が存在しない曲線状に設計されている。たとえば、溝Ｇの断面形状は、円弧状（真円のほか楕円も含む。）（図４（ａ）参照）、二等辺三角形における頂点が丸みを帯びた二等辺状（図４（ｂ）参照）または矩形における隅角部が丸みを帯びた３辺状（図４（ｃ）参照）、または台形もしくは平行四辺形における隅角部が丸みを帯びた３辺状など、様々な形状が採用されうる。 The cross-sectional shape of the groove G is designed to be a curved shape having no bent portion. For example, the cross-sectional shape of the groove G is an arc shape (including an ellipse in addition to a perfect circle) (see FIG. 4A), an isosceles shape with rounded vertices in an isosceles triangle (see FIG. 4B). ) Or a three-sided shape with rounded corners in a rectangle (see FIG. 4C), or a three-sided shape with rounded corners in a trapezoid or parallelogram sell.
接合領域における溝Ｇの面積占有率が０．２〜４５％の範囲に含まれるように当該溝Ｇが形成される。溝Ｇは、その幅ｗが０．０１〜０．５［ｍｍ］の範囲に収まり、その深さｄが０．４ｗ〜１．０ｗの範囲に収まるように設計される。 The groove G is formed so that the area occupation ratio of the groove G in the bonding region is included in the range of 0.2 to 45%. The groove G is designed such that its width w falls within the range of 0.01 to 0.5 [mm] and its depth d falls within the range of 0.4 w to 1.0 w.
（３）スラリー付着工程
図１（３）に示されているように、複数のセラミックス成形体Ｃ１およびＣ２の接合領域にスラリーＳを付着させる。スラリーＳは、セラミックス成形体Ｃ１およびＣ２と同一組成のセラミックス粉末が分散されているように調整される。分散剤としては、ポリカルボン酸アンモニウム等の一般的なものが用いられる。スラリー付着方法としては、刷毛塗り、スプレー塗布または浸漬等の一般的手法が採用される。
(3) Slurry attachment process As shown in Drawing 1 (3), slurry S is made to adhere to the joined field of a plurality of ceramic fabrication objects C1 and C2. The slurry S is adjusted so that ceramic powders having the same composition as the ceramic molded bodies C1 and C2 are dispersed. As the dispersant, a common one such as ammonium polycarboxylate is used. As a slurry adhesion method, a general method such as brush coating, spray coating, or dipping is employed.
（４）接合工程
図１（４）に示されているように、複数のセラミックス成形体Ｃ１およびＣ２を接合領域において接合させることで接合成形体Ｃが得られる。この際、接合領域を含む平面の法線方向について、セラミックス成形体Ｃ１およびＣ２に対して圧力が加えられてもよい。当該接合面同士が摺り合わせられるように、セラミックス成形体Ｃ１およびＣ２のうち一方または両方が動かされてもよい。
(4) Joining Step As shown in FIG. 1 (4), a joined compact C is obtained by joining a plurality of ceramic compacts C1 and C2 in the joint region. At this time, pressure may be applied to the ceramic molded bodies C1 and C2 in the normal direction of the plane including the bonding region. One or both of the ceramic molded bodies C1 and C2 may be moved so that the joint surfaces are slid together.
一のセラミックス成形体Ｃ１の一の面の全部と、他のセラミックス成形体Ｃ２の他の面の全部とが接合することにより接合領域が構成されていてもよく、一のセラミックス成形体Ｃ１の一の面の一部と、他のセラミックス成形体Ｃ２の他の面の一部または全部とが接合することにより接合領域が構成されていてもよい。たとえば、一のセラミックス成形体Ｃ１の上面に凹部Ｒ１が形成される一方（図３（ａ）左側参照）、他のセラミックス成形体Ｃ２の下面が平面である場合、セラミックス成形体Ｃ１およびＣ２の接合領域は、セラミックス成形体Ｃ１の上面領域（凹部Ｒ１を除く）と同じ形状になる。 A joining region may be configured by joining all of one surface of one ceramic molded body C1 and all other surfaces of another ceramic molded body C2, and one of the one ceramic molded body C1 may be formed. The joining region may be configured by joining a part of the surface and a part or all of the other surface of the other ceramic molded body C2. For example, when the concave portion R1 is formed on the upper surface of one ceramic molded body C1 (see the left side of FIG. 3A), and the lower surface of the other ceramic molded body C2 is a plane, the ceramic molded bodies C1 and C2 are joined. The region has the same shape as the upper surface region (excluding the recess R1) of the ceramic molded body C1.
（５）焼結工程
図１（５）に示されているように、接合成形体Ｃを焼結することにより一体化させてセラミックス焼結体ＳＣが得られる。
(5) Sintering Step As shown in FIG. 1 (5), the sintered compact SC is obtained by integrating the sintered compact C by sintering.
(セラミックス焼結体の構成)
図３（ａ）に示されているように凹部Ｒ１およびＲ２が形成されているセラミックス成形体Ｃ１およびＣ２により構成された接合成形体Ｃが焼成されることにより、図５（ａ）に示されているように、当該凹部Ｒ１およびＲ２によって構成される外部に連通する内部空間Ｒを有するセラミックス焼結体ＳＣが製造される。図５（ｂ）に示されているように、内部空間Ｒを画定する焼結体ＳＣの側壁には溝Ｇからはみ出したスラリーに由来する局所的な凸部Ｐが形成されている。
(Configuration of ceramic sintered body)
As shown in FIG. 3 (a), the bonded molded body C constituted by the ceramic molded bodies C1 and C2 in which the recesses R1 and R2 are formed is fired, so that it is shown in FIG. 5 (a). As described above, the ceramic sintered body SC having the internal space R communicating with the outside constituted by the recesses R1 and R2 is manufactured. As shown in FIG. 5B, local protrusions P derived from the slurry protruding from the grooves G are formed on the side walls of the sintered body SC that defines the internal space R.
内部空間Ｒを画定する側壁に対するブラスト加工等の加工が困難である場合、このような凸部が残存するが、当該加工が可能である場合には凸部が除去されてもよい。内部空間Ｒの形状は焼結体ＳＣの外部への連通箇所において断面積が小さいまたは幅狭である一方、焼結体ＳＣの内部において断面積が大きいまたは幅広である場合、当該内部における凸部の除去加工は困難であるため、焼結体ＳＣに凸部が残存する。 When processing such as blasting on the side wall that defines the internal space R is difficult, such a convex portion remains, but when the processing is possible, the convex portion may be removed. The shape of the internal space R has a small or narrow cross-sectional area at a location where the sintered body SC communicates with the outside, whereas if the cross-sectional area is large or wide inside the sintered body SC, the convex portion in the inside Since the removal process is difficult, convex portions remain in the sintered body SC.
（実施例）
（実施例１）
バインダ（製品名：バインドセラム）が添加された市販のアルミナ粉末（平均粒径０．９［μｍ］、純度９９．７％）が原料粉末としてＣＩＰ成形されることにより一の成形体が得られた。バインダの添加量は５質量％に調節された。当該一の成形体から略矩形板状の２つの成形体Ｃ１およびＣ２が切り出された。
(Example)
(Example 1)
A commercially available alumina powder (average particle size 0.9 [μm], purity 99.7%) to which a binder (product name: bind serum) is added is CIP-molded as a raw material powder to obtain a single molded body. It was. The amount of the binder added was adjusted to 5% by mass. Two molded bodies C1 and C2 having a substantially rectangular plate shape were cut out from the one molded body.
図２（ａ）に示されているように一方の成形体Ｃ１の上面に溝Ｇが形成され、その幅ｗが０．０１［ｍｍ］に調節され、その深さｄが０．００５［ｍｍ］（＝０．５０ｗ）に調節された。溝Ｇの断面形状は真円弧状に調節された。溝Ｇの接合領域における面積占有率は０．５％に調節された。 As shown in FIG. 2A, a groove G is formed on the upper surface of one molded body C1, its width w is adjusted to 0.01 [mm], and its depth d is 0.005 [mm]. ] (= 0.50 w). The cross-sectional shape of the groove G was adjusted to a true arc shape. The area occupation ratio in the junction region of the groove G was adjusted to 0.5%.
原料粉末と同じセラミックス粉末に対して、バインダに加えて分散剤およびイオン交換水が添加されることによりスラリーが調整された。接合成形体Ｃに対して、当該接合方向に０．００５［ｋｇｆ／ｃｍ2］の圧力が印加された。接合成形体Ｃが大気雰囲気で１５００〜１６５０［℃］に含まれる温度で焼成されることにより実施例１のセラミックス焼結体ＳＣが得られた。 A slurry was prepared by adding a dispersant and ion-exchanged water to the same ceramic powder as the raw material powder in addition to the binder. A pressure of 0.005 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. The sintered compact SC of Example 1 was obtained by firing the bonded compact C at a temperature included in 1500 to 1650 [° C.] in an air atmosphere.
（実施例２）
平均粒径２．０［μｍ］、純度９５．０％のアルミナ粉末が原料粉末として用いられ、バインダの添加量が４質量％に調節された。溝Ｇの幅ｗが０．５［ｍｍ］に調節され、深さｄが０．４［ｍｍ］(＝０．８ｗ)に調節された。溝Ｇの断面形状は隅角部が丸みを帯びた矩形に調節された。溝Ｇの接合領域における面積占有率は４０％に調節された。その他は実施例１と同様の条件下で実施例２のセラミックス焼結体ＳＣが得られた。
(Example 2)
An alumina powder having an average particle size of 2.0 [μm] and a purity of 95.0% was used as a raw material powder, and the amount of binder added was adjusted to 4% by mass. The width w of the groove G was adjusted to 0.5 [mm], and the depth d was adjusted to 0.4 [mm] (= 0.8 w). The cross-sectional shape of the groove G was adjusted to a rectangle with rounded corners. The area occupation ratio in the junction region of the groove G was adjusted to 40%. Otherwise, a ceramic sintered body SC of Example 2 was obtained under the same conditions as in Example 1.
（実施例３）
平均粒径０．１［μｍ］、純度９９．９％のアルミナ粉末が料粉末として用いられ、バインダの添加量が８質量％に調節された。溝Ｇの幅ｗが０．２［ｍｍ］に調節され、深さｄが０．２［ｍｍ］(＝１．０ｗ)に調節された。溝Ｇの断面形状は隋円弧状に調節された。溝Ｇの接合領域における面積占有率は２０％に調節された。接合成形体Ｃに対して当該接合方向に０．０３［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で実施例３のセラミックス焼結体ＳＣが得られた。
Example 3
An alumina powder having an average particle size of 0.1 [μm] and a purity of 99.9% was used as a powder, and the amount of binder added was adjusted to 8% by mass. The width w of the groove G was adjusted to 0.2 [mm], and the depth d was adjusted to 0.2 [mm] (= 1.0 w). The cross-sectional shape of the groove G was adjusted to be a circular arc shape. The area occupation ratio in the junction region of the groove G was adjusted to 20%. A pressure of 0.03 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Example 3 was obtained under the same conditions as in Example 1.
（実施例４）
平均粒径１．５［μｍ］、純度９６．０％のアルミナ 平均粒径０．１［μｍ］、純度９９．９％のアルミナ粉末が料粉末として用いられ、バインダの添加量が８質量％に調節された。溝Ｇの幅ｗが０．３［ｍｍ］に調節され、深さｄが０．１５［ｍｍ］(＝０．５ｗ)に調節された。溝Ｇの断面形状は真円弧状に調節された。溝Ｇの接合領域における面積占有率は０．２％に調節された。接合成形体Ｃに対して、当該接合方向に０．０５５［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で実施例４のセラミックス焼結体ＳＣが得られた。
Example 4
Alumina powder having an average particle diameter of 1.5 [μm] and a purity of 96.0% An alumina powder having an average particle diameter of 0.1 [μm] and a purity of 99.9% is used as a powder, and the amount of binder added is 8% by mass. Adjusted to. The width w of the groove G was adjusted to 0.3 [mm], and the depth d was adjusted to 0.15 [mm] (= 0.5 w). The cross-sectional shape of the groove G was adjusted to a true arc shape. The area occupancy in the junction region of the groove G was adjusted to 0.2%. A pressure of 0.055 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, the ceramic sintered body SC of Example 4 was obtained under the same conditions as in Example 1.
（実施例５）
市販のジルコニア粉末（平均粒径０．５［μｍ］）が原料粉末として用いられ、バインダ添加量が８質量％に調節された。溝Ｇの幅ｗが０．２［ｍｍ］に調節され、その深さｄが０．１４［ｍｍ］(＝０．７Ｗ)に調節された。溝Ｇの断面形状は頂点に丸みの帯びた二等辺三角形に調節された。溝Ｇの接合領域における面積占有率は４５％に調節された。接合成形体Ｃに対して、当該接合方向に０．０７０［ｋｇｆ／ｃｍ2］の圧力が印加された。接合成形体Ｃが大気雰囲気で１３５０〜１５５０［℃］に含まれる温度で焼成されることにより実施例５のセラミックス焼結体ＳＣが得られた。
(Example 5)
Commercially available zirconia powder (average particle size 0.5 [μm]) was used as a raw material powder, and the amount of binder added was adjusted to 8 mass%. The width w of the groove G was adjusted to 0.2 [mm], and the depth d was adjusted to 0.14 [mm] (= 0.7 W). The cross-sectional shape of the groove G was adjusted to an isosceles triangle with a rounded apex. The area occupation ratio in the junction region of the groove G was adjusted to 45%. A pressure of 0.070 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. The sintered compact SC of Example 5 was obtained by firing the bonded compact C at a temperature included in 1350 to 1550 [° C.] in an air atmosphere.
（実施例６）
市販の炭化珪素粉末（平均粒径１．０［μｍ］）が原料粉末として用いられた。溝Ｇの幅ｗが０．０１［ｍｍ］に調節され、その深さｄが０．００４［ｍｍ］(＝０．４ｗ)に調節された。溝Ｇの断面形状は隅角部が丸みを帯びた台形に調節された。溝Ｇの接合領域における面積占有率は１０％に調節された。接合成形体Ｃに対して、当該接合方向に０．０１６［ｋｇｆ／ｃｍ2］の圧力が印加された。接合成形体Ｃが真空を含む非酸化雰囲気で１８００〜２１００［℃］に含まれる温度で焼成されることにより実施例６のセラミックス焼結体ＳＣが得られた。
(Example 6)
Commercially available silicon carbide powder (average particle size 1.0 [μm]) was used as the raw material powder. The width w of the groove G was adjusted to 0.01 [mm], and the depth d was adjusted to 0.004 [mm] (= 0.4 w). The cross-sectional shape of the groove G was adjusted to a trapezoid with rounded corners. The area occupation ratio in the bonding region of the groove G was adjusted to 10%. A pressure of 0.016 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. The sintered compact SC of Example 6 was obtained by firing the bonded compact C at a temperature included in 1800 to 2100 [° C.] in a non-oxidizing atmosphere including vacuum.
（試験方法）
各実施例の焼結体を対象として超音波デジタル映像探傷装置（ＳＯＮＩＸ社製）により得られた探傷画像のうち、傷部分（隙間部分）を除く部分の面積の当該探傷画像の全面積に対する比率が接合率として測定された。焼結体の曲げ強度（４点曲げ強度）が測定され、成形体がそのまま焼結されることにより得られた無垢の緻密質セラミックス焼結体の曲げ強度（たとえばアルミナは４００［ＭＰａ］、ジルコニアは１０００［ＭＰａ］）を基準とする当該測定結果の低減度が測定された。３０個の試料を対象とする当該低減度の測定結果のばらつきを表わす分散σが測定された。
(Test method)
Of the flaw detection images obtained by the ultrasonic digital video flaw detector (manufactured by SONIX) for the sintered body of each example, the ratio of the area of the portion excluding the flaw portion (gap portion) to the total area of the flaw detection image Was measured as the bonding rate. The bending strength (four-point bending strength) of the sintered body was measured, and the bending strength of a pure dense ceramic sintered body obtained by sintering the formed body as it is (for example, 400 [MPa] for alumina, zirconia) Was measured based on 1000 [MPa]). The dispersion σ representing the variation in the measurement results of the degree of reduction for 30 samples was measured.
表１には、各実施例のセラミックス焼結体についてもとになったセラミックス成形体およびそこに形成された溝の態様とともに、これらの測定結果がまとめて示されている。 Table 1 summarizes the measurement results together with the ceramic molded body based on the ceramic sintered body of each example and the mode of the grooves formed therein.
表１から明らかなように、実施例１〜６のセラミックス焼結体の接合率は９０〜１００％であり、特に実施例３、４および６のセラミックス焼結体の接合率は９６％以上と高い。実施例１〜６のセラミックス焼結体の無垢材に対する曲げ強度の低減率は１０〜４０％であり、特に実施例３、４および６のセラミックス焼結体の無垢材に対する曲げ強度の低減率は２２％以下と低い。 As is apparent from Table 1, the bonding rate of the ceramic sintered bodies of Examples 1 to 6 is 90 to 100%, and in particular, the bonding rate of the ceramic sintered bodies of Examples 3, 4 and 6 is 96% or more. high. The reduction rate of the bending strength with respect to the solid material of the ceramic sintered bodies of Examples 1 to 6 is 10 to 40%. In particular, the reduction rate of the bending strength with respect to the solid material of the ceramic sintered bodies of Examples 3, 4 and 6 is It is as low as 22% or less.
（比較例）
（比較例１）
平均粒径１．０［μｍ］、純度９９．７％のアルミナ粉末が原料粉末として用いられた。溝Ｇの幅ｗが５．０［ｍｍ］に調節され、深さｄが２．５［ｍｍ］に調節された。溝Ｇの接合領域における面積占有率は４０％に調節された。その他は実施例１と同様の条件下で比較例１のセラミックス焼結体ＳＣが得られた。溝Ｇの幅ｗおよび深さｄが大きすぎるため、これがスラリーにより充填されず、接合界面に隙間の存在が確認された。
(Comparative example)
(Comparative Example 1)
An alumina powder having an average particle size of 1.0 [μm] and a purity of 99.7% was used as a raw material powder. The width w of the groove G was adjusted to 5.0 [mm], and the depth d was adjusted to 2.5 [mm]. The area occupation ratio in the junction region of the groove G was adjusted to 40%. Otherwise, a ceramic sintered body SC of Comparative Example 1 was obtained under the same conditions as in Example 1. Since the width w and depth d of the groove G were too large, it was not filled with the slurry, and the presence of a gap at the bonding interface was confirmed.
（比較例２）
平均粒径０．５［μｍ］、純度９０．０％のアルミナ粉末が原料粉末として用いられ、バインダの添加量が８質量％に調節された。溝Ｇの幅ｗが０．４［ｍｍ］に調節され、深さｄが０．２［ｍｍ］に調節された。溝Ｇの断面形状は隋円弧状に調節された。溝Ｇの接合領域における面積占有率は７０％に調節された。接合成形体Ｃに対して、当該接合方向に０．０２０［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例２のセラミックス焼結体ＳＣが得られた。溝Ｇの面積占有率が高いため、これがスラリーにより充填されず、接合界面に多数の隙間の存在が確認された。
(Comparative Example 2)
An alumina powder having an average particle size of 0.5 [μm] and a purity of 90.0% was used as a raw material powder, and the amount of binder added was adjusted to 8% by mass. The width w of the groove G was adjusted to 0.4 [mm], and the depth d was adjusted to 0.2 [mm]. The cross-sectional shape of the groove G was adjusted to be a circular arc shape. The area occupation ratio in the junction region of the groove G was adjusted to 70%. A pressure of 0.020 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 2 was obtained under the same conditions as in Example 1. Since the area occupation ratio of the groove G was high, it was not filled with the slurry, and it was confirmed that there were many gaps at the joint interface.
（比較例３）
平均粒径２．０［μｍ］、純度９８．０％のアルミナ粉末が原料粉末として用いられた。成形体Ｃ１およびＣ２のいずれにも溝Ｇは形成されず、接合成形体Ｃに対して、当該接合方向に０．０７０［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例３のセラミックス焼結体ＳＣが得られた。接合時に成形体Ｃ１およびＣ２の滑りが確認され、得られた焼結体ＳＣの接合率、強度の低下が確認された。
(Comparative Example 3)
An alumina powder having an average particle size of 2.0 [μm] and a purity of 98.0% was used as a raw material powder. The groove G was not formed in any of the molded bodies C1 and C2, and a pressure of 0.070 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 3 was obtained under the same conditions as in Example 1. Slip of the compacts C1 and C2 was confirmed at the time of joining, and a reduction in joining rate and strength of the obtained sintered body SC was confirmed.
（比較例４）
平均粒径０．８［μｍ］、純度９５．５％のアルミナ粉末が原料粉末として用いられた。図２（ｂ）に示されているように成形体Ｃ１およびＣ２のそれぞれに溝Ｇが形成され、その幅ｗが０．５［ｍｍ］に調節され、その深さｄが０．２５［ｍｍ］に調節された。溝Ｇの断面形状が二等辺三角形の二等辺形状（Ｖ字形状）に調節された。溝Ｇの接合領域における面積占有率は３０％に調節された。接合成形体Ｃに対して、当該接合方向に０．００８［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例４のセラミックス焼結体ＳＣが得られた。溝Ｇの断面形状が屈曲箇所を有するため、接合界面に隙間およびクラックが発生した。
(Comparative Example 4)
An alumina powder having an average particle size of 0.8 [μm] and a purity of 95.5% was used as a raw material powder. As shown in FIG. 2B, a groove G is formed in each of the molded bodies C1 and C2, its width w is adjusted to 0.5 [mm], and its depth d is 0.25 [mm]. ] Was adjusted. The cross-sectional shape of the groove G was adjusted to an isosceles triangle isosceles shape (V shape). The area occupation ratio in the junction region of the groove G was adjusted to 30%. A pressure of 0.008 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 4 was obtained under the same conditions as in Example 1. Since the cross-sectional shape of the groove G has a bent portion, a gap and a crack occurred at the bonding interface.
（比較例５）
平均粒径１．２［μｍ］、純度９８．０％のアルミナ粉末が原料粉末として用いられた。図２（ｂ）に示されているように成形体Ｃ１およびＣ２のそれぞれに溝Ｇが形成され、その幅ｗが０．５［ｍｍ］に調節され、その深さｄが５．０［ｍｍ］に調節された。溝Ｇの断面形状は隋円弧状に調節された。溝Ｇの接合領域における面積占有率は１０％に調節された。接合成形体Ｃに対して、当該接合方向に０．０１０［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例５のセラミックス焼結体ＳＣが得られた。溝Ｇの深さｄが大きく、アスペクト比の高い溝構造のため、溝Ｇを基点としたクラックが発生した。
(Comparative Example 5)
An alumina powder having an average particle size of 1.2 [μm] and a purity of 98.0% was used as a raw material powder. As shown in FIG. 2B, a groove G is formed in each of the molded bodies C1 and C2, its width w is adjusted to 0.5 [mm], and its depth d is 5.0 [mm]. ] Was adjusted. The cross-sectional shape of the groove G was adjusted to be a circular arc shape. The area occupation ratio in the bonding region of the groove G was adjusted to 10%. A pressure of 0.010 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 5 was obtained under the same conditions as in Example 1. Due to the groove structure having a large depth d and a high aspect ratio, cracks with the groove G as a starting point occurred.
（比較例６）
平均粒径０．８［μｍ］、純度９５．０％のアルミナ粉末が原料粉末として用いられ、バインダの添加量が８質量％に調節された。溝Ｇの幅ｗが０．４［ｍｍ］に調節され、深さｄが０．１［ｍｍ］に調節された。溝Ｇの断面形状は隋円弧状に調節された。溝Ｇの接合領域における面積占有率は３０％に調節された。接合成形体Ｃに対して、当該接合方向に０．０２０［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例６のセラミックス焼結体ＳＣが得られた。成形体同士の接合時にスラリーの潤滑作用による滑りが確認された。
(Comparative Example 6)
An alumina powder having an average particle size of 0.8 [μm] and a purity of 95.0% was used as a raw material powder, and the amount of binder added was adjusted to 8% by mass. The width w of the groove G was adjusted to 0.4 [mm], and the depth d was adjusted to 0.1 [mm]. The cross-sectional shape of the groove G was adjusted to be a circular arc shape. The area occupation ratio in the junction region of the groove G was adjusted to 30%. A pressure of 0.020 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 6 was obtained under the same conditions as in Example 1. Sliding due to the lubricating action of the slurry was confirmed when the compacts were joined.
（比較例７）
平均粒径１．０［μｍ］、純度９２．０％のアルミナ粉末が原料粉末として用いられ、バインダの添加量が５質量％に調節された。溝Ｇの幅ｗが０．００５［ｍｍ］に調節され、深さｄが０．００２５［ｍｍ］に調節された。溝Ｇの断面形状は真円弧状に調節された。溝Ｇの接合領域における面積占有率は５％に調節された。接合成形体Ｃに対して、当該接合方向に０．０３５［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例７のセラミックス焼結体ＳＣが得られた。溝幅ｗが狭すぎるため、接合時に成形体Ｃ１およびＣ２の滑りが確認され、得られた焼結体ＳＣの接合率、強度の低下が確認された。
(Comparative Example 7)
An alumina powder having an average particle size of 1.0 [μm] and a purity of 92.0% was used as a raw material powder, and the amount of binder added was adjusted to 5% by mass. The width w of the groove G was adjusted to 0.005 [mm], and the depth d was adjusted to 0.0025 [mm]. The cross-sectional shape of the groove G was adjusted to a true arc shape. The area occupation ratio in the junction region of the groove G was adjusted to 5%. A pressure of 0.035 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 7 was obtained under the same conditions as in Example 1. Since the groove width w was too narrow, slipping of the molded bodies C1 and C2 was confirmed at the time of joining, and a reduction in the joining rate and strength of the obtained sintered body SC was confirmed.
（比較例８）
平均粒径０．５［μｍ］、純度９０．０％のアルミナ粉末が原料粉末として用いられ、バインダの添加量が５質量％に調節された。溝Ｇの幅ｗが０．２［ｍｍ］に調節され、深さｄが０．１２［ｍｍ］に調節された。溝Ｇの断面形状は隋円弧状に調節された。溝Ｇの接合領域における面積占有率は０．１％に調節された。接合成形体Ｃに対して、当該接合方向に０．０１６［ｋｇｆ／ｃｍ2］の圧力が印加された。その他は実施例１と同様の条件下で比較例８のセラミックス焼結体ＳＣが得られた。溝Ｇの面積占有率が少ないため、接合時に成形体Ｃ１およびＣ２の滑りが確認され、得られた焼結体ＳＣの接合率、強度の低下が確認された。
(Comparative Example 8)
An alumina powder having an average particle size of 0.5 [μm] and a purity of 90.0% was used as a raw material powder, and the amount of binder added was adjusted to 5% by mass. The width w of the groove G was adjusted to 0.2 [mm], and the depth d was adjusted to 0.12 [mm]. The cross-sectional shape of the groove G was adjusted to be a circular arc shape. The area occupation ratio in the junction region of the groove G was adjusted to 0.1%. A pressure of 0.016 [kgf / cm 2 ] was applied to the bonded molded body C in the bonding direction. Otherwise, a ceramic sintered body SC of Comparative Example 8 was obtained under the same conditions as in Example 1. Since the area occupancy of the groove G is small, slipping of the molded bodies C1 and C2 was confirmed during bonding, and a decrease in the bonding ratio and strength of the obtained sintered body SC was confirmed.
表２には、各比較例のセラミックス焼結体についてもとになったセラミックス成形体およびそこに形成された溝の態様とともに、これらの測定結果がまとめて示されている。 Table 2 summarizes the measurement results together with the ceramic molded body based on the ceramic sintered bodies of the comparative examples and the mode of the grooves formed therein.
表２から明らかなように、比較例１〜８のセラミックス焼結体の接合率は７６〜８９％であり、実施例１〜６のセラミックス焼結体の接合率と比較して低い。比較例１〜８のセラミックス焼結体の無垢材に対する曲げ強度の低減率は４５〜６２％であり、実施例１〜６のセラミックス焼結体の無垢材に対する曲げ強度の低減率よりも高い。 As is apparent from Table 2, the bonding rate of the ceramic sintered bodies of Comparative Examples 1 to 8 is 76 to 89%, which is lower than the bonding rate of the ceramic sintered bodies of Examples 1 to 6. The reduction rate of the bending strength of the ceramic sintered bodies of Comparative Examples 1 to 8 with respect to the solid material is 45 to 62%, which is higher than the reduction rate of the bending strength of the ceramic sintered bodies of Examples 1 to 6 with respect to the solid material.
Ｃ‥接合成形体、Ｃ１、Ｃ２‥複数のセラミックス成形体、Ｇ‥溝、Ｐ‥凸部、Ｒ‥閉塞内部空間、Ｓ‥スラリー、ＳＣ‥セラミックス焼結体。 C: Bonded molded body, C1, C2: Multiple ceramic molded bodies, G: Groove, P: Convex part, R: Closure internal space, S: Slurry, SC: Ceramic sintered body
Claims (3)
前記複数のセラミックス成形体のうち少なくとも１つに、前記複数のセラミックス成形体同士の接合領域から当該接合領域の境界まで連続する幅０．０１〜０．５［ｍｍ］かつ当該幅の０．４〜１．０倍の深さの、屈曲箇所が存在しない曲線状の断面形状を有するような溝を形成する工程と、
前記複数のセラミックス成形体と同一組成のセラミックス粉末が分散されているスラリーを前記接合領域に付着させる工程と、
前記複数のセラミックス成形体同士を前記接合領域において接合させる工程と、
当該接合された前記複数のセラミックス成形体を焼結して一体化する工程と、を含むセラミックス焼結体の製造方法。 Preparing a plurality of ceramic molded bodies having the same composition;
At least one of the plurality of ceramic compacts has a width of 0.01 to 0.5 [mm] continuous from the joint region between the ceramic compacts to the boundary of the joint region, and 0.4 of the width. A step of forming a groove having a curved cross-sectional shape with no bent portion at a depth of -1.0 times;
Attaching a slurry in which ceramic powder having the same composition as the plurality of ceramic molded bodies is dispersed to the joining region;
Bonding the plurality of ceramic molded bodies to each other in the bonding region;
A step of sintering and integrating the plurality of joined ceramic molded bodies.
前記内部空間を画定する側壁に前記溝からはみ出した前記スラリーに由来する局所的な凸部が形成されているセラミックス焼結体。 A ceramic sintered body produced by the method according to claim 1 or 2 and having an internal space communicating with the outside,
The ceramic sintered compact by which the local convex part derived from the said slurry protruded from the said groove | channel is formed in the side wall which demarcates the said internal space.
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| KR20200024910A (en) | 2017-08-29 | 2020-03-09 | 쿄세라 코포레이션 | Ceramic assembly and its manufacturing method |
| JP2020138877A (en) * | 2019-02-27 | 2020-09-03 | 京セラ株式会社 | Member for semiconductor production device, and method of producing the same |
| US11999660B2 (en) | 2017-08-29 | 2024-06-04 | Kyocera Corporation | Ceramic joined body and method for manufacturing same |
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| JP2011011930A (en) * | 2009-06-30 | 2011-01-20 | Taiheiyo Cement Corp | Method for producing ceramic sintered compact |
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| KR20200024910A (en) | 2017-08-29 | 2020-03-09 | 쿄세라 코포레이션 | Ceramic assembly and its manufacturing method |
| US11999660B2 (en) | 2017-08-29 | 2024-06-04 | Kyocera Corporation | Ceramic joined body and method for manufacturing same |
| JP2020138877A (en) * | 2019-02-27 | 2020-09-03 | 京セラ株式会社 | Member for semiconductor production device, and method of producing the same |
| JP7181123B2 (en) | 2019-02-27 | 2022-11-30 | 京セラ株式会社 | Member for semiconductor manufacturing equipment and manufacturing method thereof |
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