JP6335737B2 - Method for producing hollow structure - Google Patents
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- JP6335737B2 JP6335737B2 JP2014200434A JP2014200434A JP6335737B2 JP 6335737 B2 JP6335737 B2 JP 6335737B2 JP 2014200434 A JP2014200434 A JP 2014200434A JP 2014200434 A JP2014200434 A JP 2014200434A JP 6335737 B2 JP6335737 B2 JP 6335737B2
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- 238000004519 manufacturing process Methods 0.000 title description 12
- 239000000919 ceramic Substances 0.000 claims description 69
- 239000007767 bonding agent Substances 0.000 claims description 50
- 238000000034 method Methods 0.000 claims description 14
- 230000003746 surface roughness Effects 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 3
- 238000005304 joining Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000001154 acute effect Effects 0.000 description 2
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 2
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
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- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 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
- 230000009466 transformation Effects 0.000 description 1
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- Ceramic Products (AREA)
- Compositions Of Oxide Ceramics (AREA)
Description
本発明は、セラミックス焼結体から構成されている中空構造体の製造方法に関する。 The present invention relates to the production how hollow structure and a ceramic sintered body.
半導体製造装置に用いられるセラミックス部材は、その内部に冷媒等の熱媒体が流通可能な溝などの複雑な構造の中空部を設ける必要がある場合がある。このような場合、外からの加工で中空部を設けることはできず、予め中空部となる溝を形成したセラミックス成形体を接合して焼成することによって、中空構造部を有するセラミックス部材を得ている。 A ceramic member used in a semiconductor manufacturing apparatus may need to be provided with a hollow portion having a complicated structure such as a groove through which a heat medium such as a refrigerant can flow. In such a case, a hollow part cannot be provided by processing from the outside, and a ceramic member having a hollow structure part is obtained by joining and firing a ceramic molded body in which a groove that becomes a hollow part is formed in advance. Yes.
従来、例えば特許文献１には、セラミックス成形体の研磨した各接合面にエタノールを塗布し、これら接合面を合わせた面に共素地泥しょうを流し込んで隙間を埋め、乾燥させて接合した後に焼結することが提案されている。 Conventionally, for example, in Patent Document 1, ethanol is applied to each polished joint surface of a ceramic molded body, and a common ground mud is poured into a surface where these joint surfaces are combined to fill gaps, which are dried and joined. It has been proposed to conclude.
また、例えば特許文献２には、セラミックス部材と同材質からなる粉体と樹脂とを溶媒で混合したスラリーをセラミックス成形体の接合面に塗布し、セラミックス成形体の接合面同士を当接させた状態で乾燥させて接合した後に焼成することが提案されている。 Also, for example, in Patent Document 2, a slurry obtained by mixing a powder made of the same material as a ceramic member and a resin with a solvent is applied to the bonding surface of the ceramic molded body, and the bonded surfaces of the ceramic molded body are brought into contact with each other. It has been proposed to fire after drying and joining in a state.
しかしながら、特許文献１，２に記載の技術では、セラミックス成形体の接合面は研磨加工されているが、接合面と中空構造部の境界部分の端面は加工されておらず、角張った形状となっている。特に、特許文献２の図面では、この部分は直角に近い角張った形状であり、端面は何ら加工されていない。 However, in the techniques described in Patent Documents 1 and 2, the bonding surface of the ceramic molded body is polished, but the end surface of the boundary portion between the bonding surface and the hollow structure portion is not processed and has an angular shape. ing. In particular, in the drawing of Patent Document 2, this portion has an angular shape close to a right angle, and the end face is not processed at all.
このように境界部分が角張った形状の場合、セラミックス成形体を当接した際に染み出た接合剤が中空構造部の側面に流れ、そのまま密着して乾燥固化する。染み出した接合剤を除去するために、中空構造部内を水などの溶媒で洗浄すると、乾燥が不十分であった接合剤が欠落し、未接合な部分が生じるおそれがある。さらに、接合後は中空構造部内を追加工することは困難であるため、接合剤が染み出して固着したまま焼成せざるを得ない。中空構造部に接合剤が染み出して固着した箇所があると、中空構造部内を流れる熱媒体に由来して堆積物（スケール）の付着が進むという問題がある。 In the case where the boundary portion has an angular shape as described above, the bonding agent that has oozed out when the ceramic molded body comes into contact flows to the side surface of the hollow structure portion, and adheres as it is to be dried and solidified. If the inside of the hollow structure portion is washed with a solvent such as water in order to remove the bonding agent that has oozed out, the bonding agent that has not been sufficiently dried may be lost, and an unbonded portion may be generated. Furthermore, since it is difficult to additionally process the inside of the hollow structure part after joining, it must be baked while the joining agent oozes out and is fixed. If there is a portion where the bonding agent oozes out and adheres to the hollow structure portion, there is a problem that the deposit (scale) adheres due to the heat medium flowing in the hollow structure portion.
そこで、本発明は、セラミックス成形体の接合時に接合面に塗布などした接合剤が中空構造部内に流れ出し難くすることを図りうる中空構造体の製造方法を提供することを目的とする。 The present invention aims to provide a manufacturing how hollow structure bonding agent and the like applied to the bonding surface at the time of bonding can strive to make it difficult flows into the hollow structure of the ceramic body.
本発明の中空構造体の製造方法は、中空構造部となる溝が接合面に形成され、前記溝と前記接合面との境界部分に、当該接合面における面取り長さが０．１０ｍｍ〜５．００ｍｍの面取り加工されたセラミックス成形体を用意する工程と、前記セラミックス成形体の溝の内面を表面粗さＲａ２．０μｍ以下に加工する工程と、前記セラミックス成形体と別のセラミックス成形体とを接合面に接合剤を介した状態で接合する工程と、前記溝の底面部分だけを溶媒で洗浄する工程と、前記接合したセラミックス成形体を焼成する工程とを備えることを特徴とする。 In the method for producing a hollow structure according to the present invention, a groove serving as a hollow structure portion is formed on a joint surface, and a chamfer length at the joint surface is 0.10 mm to 5.5 at a boundary portion between the groove and the joint surface. A step of preparing a chamfered ceramic molded body of 00 mm, a step of processing the inner surface of the groove of the ceramic molded body to a surface roughness Ra of 2.0 μm or less, and joining the ceramic molded body and another ceramic molded body It comprises a step of bonding to a surface with a bonding agent interposed therebetween, a step of cleaning only the bottom surface portion of the groove with a solvent, and a step of firing the bonded ceramic formed body.
本発明の中空構造体の製造方法によれば、接合時に接合面から接合剤が染み出しても、面取り部の接合面側の面取りされた部分の長さが０．１０ｍｍ以上と長いので、接合剤はこの部分の上に表面張力によって留まり、溝内に流れ落ちない。 According to the method for manufacturing a hollow structure of the present invention, even if the bonding agent oozes out from the bonding surface during bonding, the length of the chamfered portion on the bonding surface side of the chamfered portion is as long as 0.10 mm or more. The agent stays on this part due to surface tension and does not flow down into the groove.
また、面取り部の接合面側の面取りされた部分の長さが５．００ｍｍ以下であるので、十分な接合強度を得るために必要な接合面の面積を確保することが可能となる。 Further, since the length of the chamfered portion on the bonding surface side of the chamfered portion is 5.00 mm or less, it is possible to secure the area of the bonding surface necessary for obtaining sufficient bonding strength.
ところで、万が一、接合時に接合剤を過剰に塗布した場合、接合時に過剰な押圧力を加えた場合などには、接合面から過剰な接合剤が染み出し、面取り部だけに留まらず、中空構造部内に流れ落ちるおそれがある。 By the way, if an excessive amount of bonding agent is applied at the time of bonding, or excessive pressing force is applied at the time of bonding, excessive bonding agent oozes out from the bonding surface, and not only in the chamfered portion, but in the hollow structure portion. May flow down.
そこで、本発明の中空構造体の製造方法において、前記セラミックス成形体の溝の内面を表面粗さＲａ２．０μｍ以下に加工する工程を含む。 Therefore, the method for manufacturing a hollow structure of the present invention includes a step of processing the inner surface of the groove of the ceramic molded body to a surface roughness Ra of 2.0 μm or less .
これにより、例え、接合面から過剰な接合剤が染み出した場合であっても、溝の内側面はＲａ２．０μｍ以下と平滑であるので、接合剤は滞りなく溝の底面側に流れ落ちる。よって、溝の底面部分だけを水などの溶媒で洗浄することにより、接合層への水などの浸入、浸透などによるダメージなく、底面に溜まった染み出した接合剤の余剰分を簡便に排出することができる。 Thereby , even if excessive bonding agent oozes out from the bonding surface, the inner surface of the groove is smooth at Ra 2.0 μm or less, so that the bonding agent flows down to the bottom surface side of the groove without stagnation. Therefore, by washing only the bottom surface of the groove with a solvent such as water, the excess of the bonding agent that has oozed out on the bottom surface can be easily discharged without any damage caused by the penetration or penetration of water into the bonding layer. be able to.
（中空構造体の製造方法）
本発明の一実施形態としての中空構造体１０の製造方法を図１を参照して説明する。
(Method for producing hollow structure)
A method for manufacturing the hollow structure 10 as one embodiment of the present invention will be described with reference to FIG.
まず、図１（ａ）に示すように、第１セラミックス成形体１１と第２セラミックス１２とを用意する工程を行う。これらセラミックス成形体１１，１２は、アルミナ、ジルコニア、炭化珪素、窒化珪素などのセラミックスからなる成形体である。この際、セラミックス成形体１１，１２の成形方法は何ら限定されず、ＣＩＰ成形法、鋳込み成形法、押出し成形法などを適用することができる。 First, as shown to Fig.1 (a), the process which prepares the 1st ceramic molded object 11 and the 2nd ceramic 12 is performed. These ceramic compacts 11 and 12 are compacts made of ceramics such as alumina, zirconia, silicon carbide, and silicon nitride. At this time, the molding method of the ceramic molded bodies 11 and 12 is not limited at all, and a CIP molding method, a casting molding method, an extrusion molding method, or the like can be applied.
これらセラミックス成形体１１，１２は、単一のセラミックス成形体を切断して分割したものであっても、別個のセラミックス成形体からなるものであってもよい。 These ceramic molded bodies 11 and 12 may be formed by cutting and dividing a single ceramic molded body, or may be formed of separate ceramic molded bodies.
これらセラミックス成形体１１，１２のそれぞれの接合面１１ａ，１２ａに対して、ＮＣ旋盤、ＭＣ加工機などの平面研削機を用いて、表面粗さが、好ましくはＲａ８．０μｍ以下、より好ましくは２．５μｍ以下となるように平面研磨する。 Using a surface grinding machine such as an NC lathe or an MC processing machine, the surface roughness is preferably Ra 8.0 μm or less, more preferably 2 for the joint surfaces 11a and 12a of the ceramic molded bodies 11 and 12, respectively. Surface polishing so that the thickness is 5 μm or less.
さらに、これらセラミックス成形体１１，１２に、中空構造体１０の中空構造部１０ｄ（図３（ａ）参照）となる溝１１ｂ，１２ｂを、接合面１１ａ，１２ａから掘り込むようにそれぞれ形成する。なお、セラミックス成形体１１，１２の何れか一方のみに、溝１１ｂ，１２ｂを形成したものであってもよい。溝１１ｂ，１２ｂの内側面は、表面粗さがＲａ２．０μｍ以下と平滑化するように研磨加工する。 Further, grooves 11b and 12b to be hollow structure portions 10d (see FIG. 3A) of the hollow structure 10 are respectively formed in the ceramic molded bodies 11 and 12 so as to be dug from the joint surfaces 11a and 12a. In addition, you may form the groove | channels 11b and 12b only in any one of the ceramic molded bodies 11 and 12. FIG. The inner surfaces of the grooves 11b and 12b are polished so that the surface roughness is smoothed to Ra 2.0 μm or less.
さらに、図２（ａ）に示すように、これらセラミックス成形体１１，１２の、接合面１１ａ，１２ａと溝１１ｂ，１２ｂとの境界部分１１ｃ，１２ｃは、角張った形状とならないように、Ｃ面取り加工を施す。面取り部の接合面１１ａ，１２ａ側の面取りされた部分の長さ（水平方向の面取り長さ）Ｌ１は０．１０ｍｍ〜５．００ｍｍである。そして、面取り部の溝１１ｂ，１２ｂの内側面１１ｄ，１２ｄ側の面取りされた部分の長さ（垂直方向の面取り長さ）Ｌ２も０．１０ｍｍ〜５．００ｍｍである。 Further, as shown in FIG. 2 (a), the chamfered chamfers are formed so that the boundary portions 11c and 12c between the joining surfaces 11a and 12a and the grooves 11b and 12b of the ceramic molded bodies 11 and 12 do not have an angular shape. Apply processing. The length (horizontal chamfering length) L1 of the chamfered portion of the chamfered portion on the side of the joint surfaces 11a and 12a is 0.10 mm to 5.00 mm. The length (vertical chamfering length) L2 of the chamfered portions of the chamfered grooves 11b and 12b on the inner side surfaces 11d and 12d side is also 0.10 mm to 5.00 mm.
なお、図２（ｂ）に示すように、境界部分１１ｃ，１２ｃは、Ｒ面取りがなされていてもよい。この場合も、面取り部の接合面１１ａ，１２ａ側の面取りされた部分の長さ（水平方向の面取り長さ）Ｌ１は０．１０ｍｍ〜５．００ｍｍである。 As shown in FIG. 2B, the boundary portions 11c and 12c may be chamfered. Also in this case, the length (horizontal chamfering length) L1 of the chamfered portion of the chamfered portion on the side of the joint surfaces 11a and 12a is 0.10 mm to 5.00 mm.
さらに、境界部分１１ｂ，１２ｂの面取りは、Ｃ面取り、Ｒ面取りに限定されず、例えば、３０度などの傾斜角を有する面取り、四分楕円形状の面取りなどであってもよい。そして、これらの場合も、面取り部の接合面１１ａ，１２ａ側の面取りされた部分の長さ（水平方向の面取り長さ）Ｌ１が０．１０ｍｍ〜５．００ｍｍであればよい。 Further, the chamfering of the boundary portions 11b and 12b is not limited to C chamfering and R chamfering, and may be chamfering having an inclination angle of 30 degrees, quadrant elliptical chamfering, and the like. In these cases as well, the length (horizontal chamfering length) L1 of the chamfered portion of the chamfered portion on the side of the joint surfaces 11a and 12a may be 0.10 mm to 5.00 mm.
また、図１（ａ）に示すように、溝１１ｂ，１２ｂの縦断面において、鋭角、鈍角など角度に関係なく、底の隅部１１ｅ，１２ｅには、隅Ｒが０．１０ｍｍ〜５０．００ｍｍのＲ隅加工を施す。 Further, as shown in FIG. 1A, in the longitudinal section of the grooves 11b and 12b, the corners 11e and 12e have corners R of 0.10 mm to 50.00 mm regardless of angles such as acute angles and obtuse angles. The R corner is processed.
次に、図１（ｂ）に示すように、セラミックス成形体１１，１２のそれぞれの接合面１１ａ，１２ａとの間に接合剤１３を介在させた状態とする。 Next, as shown in FIG. 1B, the bonding agent 13 is interposed between the bonding surfaces 11a and 12a of the ceramic molded bodies 11 and 12, respectively.
接合剤１３は、例えば、上記特許文献２に記載されたように、セラミックス成形体１１，１２材と同材質からなる粉体と樹脂とを溶媒で混合したスラリーであってもよい。この場合、接合剤１３を接合面１１ａ，１１ａに噴霧、塗布する、あるいは、接合剤１３中にセラミックス成形体１１，１２を浸漬するなどした後、セラミックス成形体１１，１２の接合面１１ａ，１２ａ同士を当接した状態とする。 For example, as described in Patent Document 2, the bonding agent 13 may be a slurry in which a powder made of the same material as the ceramic molded bodies 11 and 12 and a resin are mixed with a solvent. In this case, the bonding agent 13 is sprayed and applied to the bonding surfaces 11 a and 11 a, or the ceramic molded bodies 11 and 12 are immersed in the bonding agent 13, and then the bonding surfaces 11 a and 12 a of the ceramic molded bodies 11 and 12. It is set as the state which mutually contacted.
なお、接合剤１３は、上記特許文献１に記載されたように、エタノール及び共素地泥しょうからなるものなどであってもよい。 In addition, the bonding agent 13 may be composed of ethanol and selenium clay as described in Patent Document 1 above.
そして、セラミックス成形体１１，１２の接合面１１ａ，１２ａ間に接合剤１３を介在させた状態で乾燥させて接合する工程を行う。 And the process of drying and joining in the state which interposed the bonding agent 13 between the joining surfaces 11a and 12a of the ceramic molded bodies 11 and 12 is performed.
そして、接合させたセラミックス成形体１１，１２を、大気中で１５００℃以上の温度で焼成して接合する工程を行う。これにより、図３（ａ）に示すように中空構造体１０を得ることができる。 And the process which baked and joined the joined ceramic molded bodies 11 and 12 at the temperature of 1500 degreeC or more in air | atmosphere is performed. Thereby, as shown to Fig.3 (a), the hollow structure 10 can be obtained.
この焼成時に、炉内の温度分布やセラミックス成形体１１，１２の密度むらなどによる中空構造体１０自体の変形や反り、セラミックス成形体１１，１２を設置する台板の歪みに伴う変形などが生じても接合剤１３とセラミックス成形体１１，１２が剥離しないように、接合層１０ｃの厚みが１０〜２５００μｍとなるように、接合剤１３の厚さを調整することが好ましい。 During this firing, deformation and warpage of the hollow structure 10 itself due to temperature distribution in the furnace and uneven density of the ceramic molded bodies 11 and 12, deformation due to distortion of the base plate on which the ceramic molded bodies 11 and 12 are installed, and the like occur. However, it is preferable to adjust the thickness of the bonding agent 13 so that the bonding layer 10c has a thickness of 10 to 2500 μm so that the bonding agent 13 and the ceramic molded bodies 11 and 12 do not peel off.
接合層１０ｃの厚さが１０μｍ以下では、接合面積が８インチを超えるなどすると、剥離や未接合が生じる傾向にある。一方、接合層１０ｃの厚さが２５００μｍ以上では、接合層１０ｃの平滑性が低下し、接合むらが生じやすい。 When the thickness of the bonding layer 10c is 10 μm or less, peeling or unbonding tends to occur when the bonding area exceeds 8 inches. On the other hand, when the thickness of the bonding layer 10c is 2500 μm or more, the smoothness of the bonding layer 10c decreases, and uneven bonding is likely to occur.
図１（ａ）及び図１（ｂ）も参照して、接合前の境界部分１１ｃ，１２ｃに面取り加工が施されているので、接合時に、接合剤１３が染み出しても、ある程度の接合剤１３は接合面１１ａ，１２ａ側の面取りされた部分の上に表面張力によって留まり、中空構造部１０ｄ内に流れ込まない。 1 (a) and 1 (b), since the chamfering is performed on the boundary portions 11c and 12c before joining, even if the joining agent 13 oozes out during joining, a certain amount of joining agent is used. 13 remains on the chamfered portion on the joint surfaces 11a and 12a side by surface tension and does not flow into the hollow structure portion 10d.
ところで、境界部分１１ｃ，１２ｃに面取り加工が施されていない場合、接合直後から中空構造部１０ｄ内への染み出しが多くなる。さらに、半導体製造装置などに使用される製品となる構造上、中空構造部１０ｄは、外部と通じているので、接合層１０ｃよりも乾燥が進み、毛管作用によって接合剤１３の連続的な染み出しが発生する。 By the way, when the chamfering process is not performed on the boundary portions 11c and 12c, the seepage into the hollow structure portion 10d increases immediately after joining. Furthermore, since the hollow structure portion 10d communicates with the outside because of the structure used as a product used in a semiconductor manufacturing apparatus or the like, the drying progresses more than the bonding layer 10c, and the continuous exudation of the bonding agent 13 by capillary action. Will occur.
境界部分１１ｃ，１２ｃに面取り加工が施されていない場合、これらの理由によって、中空構造部１０ｄ近傍に位置する接合層１０ｃは、中空構造部１０ｄから離れて位置する接合層１０ｃと比較して、厚みが薄くなる傾向がある。そのため、中空構造体１０の接合強度のばらつきが大きい。そして、前述した傾向は、中空構造体１０が大型化するほど顕著であり、極端な例では、中空構造部１０ｄ近傍の接合層１０ｃが空洞化するおそれもある。 When chamfering is not performed on the boundary portions 11c and 12c, for these reasons, the bonding layer 10c positioned in the vicinity of the hollow structure portion 10d is compared with the bonding layer 10c positioned away from the hollow structure portion 10d, The thickness tends to be thin. Therefore, the dispersion | variation in the joining strength of the hollow structure 10 is large. And the tendency mentioned above becomes so remarkable that the hollow structure 10 enlarges, and there exists a possibility that the joining layer 10c of the hollow structure part 10d vicinity may become hollow in an extreme example.
一方、本実施形態では、境界部分１１ｃ，１２ｃに面取り加工が施されているので、接合時における接合層１０ｃからの接合剤１３の染み出しが表面張力の効果によって少なくなり、接合層１０ｃの厚さのばらつきが抑制される。よって、中空構造体１０の接合強度のばらつきが低減する。 On the other hand, in this embodiment, since the boundary portions 11c and 12c are chamfered, the bleeding of the bonding agent 13 from the bonding layer 10c during bonding is reduced by the effect of surface tension, and the thickness of the bonding layer 10c. Variation in thickness is suppressed. Therefore, variation in the bonding strength of the hollow structure 10 is reduced.
そして、万が一、接合時に接合剤１３を過剰に塗布した場合、接合時に過剰な印加圧力を加えた場合などには、接合面１１ａ，１２ａから過剰な接合剤１３が染み出し、面取り部だけに留まらず、溝１１ｂ，１２ｂ内に流れ落ちるおそれがある。このような場合であっても、境界部分が面取り部であるので傾斜を有し、さらに溝１１ｂ，１２ｂの内側面１１ｄ，１２ｄは、平滑に研磨されているので、滞りなく溝１１ｂ，１２ｂの底面側に流れ落ちる。 If the bonding agent 13 is excessively applied at the time of bonding, or if an excessive applied pressure is applied at the time of bonding, the excessive bonding agent 13 oozes out from the bonding surfaces 11a and 12a and remains only at the chamfered portion. There is a risk that it will flow down into the grooves 11b and 12b. Even in such a case, since the boundary portion is a chamfered portion, it has an inclination and the inner side surfaces 11d and 12d of the grooves 11b and 12b are polished smoothly, so that the grooves 11b and 12b It flows down to the bottom side.
よって、最終的に、中空構造部１０ｄの底面部分だけを水などで洗浄することにより、接合層１０ｃへの水などの浸入、浸透などによるダメージなく、底面に溜まった染み出した接合剤１３の余剰分を簡便に排出することができる。 Therefore, finally, by washing only the bottom surface portion of the hollow structure portion 10d with water or the like, the leakage of the bonding agent 13 that has accumulated on the bottom surface without damage due to the penetration or penetration of water or the like into the bonding layer 10c. Surplus can be easily discharged.
なお、中空構造部１０ｄに接合剤１３が染み出し箇所があると、中空構造部１０ｄに流れる熱媒体に由来して堆積物（スケール）の付着が進むという問題がある。 In addition, if there is a spot where the bonding agent 13 oozes out in the hollow structure portion 10d, there is a problem that deposit (scale) adheres due to the heat medium flowing in the hollow structure portion 10d.
さらに、境界部分１１ｃ，１２ｃ及び溝１１ｂ，１２ｂの隅部１１ｅ，１２ｅが角張った形状であると、クラックが発生する要因となり易い。さらに、染み出した接合剤１３が溝１１ｂ，１２ｂの内側面１１ｄ，１２ｄに固着した状態では、セラミックス成形体１１，１２と接合剤１３との収縮挙動の差異が顕著となり、クラックが発生し易い。 Furthermore, if the boundary portions 11c and 12c and the corner portions 11e and 12e of the grooves 11b and 12b have an angular shape, it is likely to cause a crack. Further, in the state where the exuded bonding agent 13 is fixed to the inner side surfaces 11d and 12d of the grooves 11b and 12b, the difference in shrinkage behavior between the ceramic molded bodies 11 and 12 and the bonding agent 13 becomes remarkable, and cracks are likely to occur. .
しかし、本発明の中空構造体１０では、図１（ａ）に示すように境界部分１１ｃ，１２ｃに面取り加工が施され、接合剤１３の溝１１ｂ，１２ｂの内側面１１ｄ，１２ｄへの固着が防止されるので、このようなクラックが発生することを抑制することができ、歩留まりを向上させることが可能となる。 However, in the hollow structure 10 of the present invention, as shown in FIG. 1A, the boundary portions 11c and 12c are chamfered to fix the bonding agent 13 to the inner surfaces 11d and 12d of the grooves 11b and 12b. Therefore, the occurrence of such cracks can be suppressed, and the yield can be improved.
（中空構造体の構成）
本発明の一実施形態としての中空構造体１０は、図３（ａ）に示すように、第１のセラミックス焼結体部１０ａと、第２のセラミックス焼結体部１０ｂと、これらセラミックス焼結体部１０ａ，１０ｂの間に介在する接合層１０ｃとを有し、セラミックス焼結体部１０ａ，１０ｂに形成された中空構造部１０ｄに接合層１０ｃに沿って凹部１０ｅが形成されている。
(Configuration of hollow structure)
As shown in FIG. 3A, the hollow structure 10 as one embodiment of the present invention includes a first ceramic sintered body portion 10a, a second ceramic sintered body portion 10b, and a ceramic sintered body. A recess 10e is formed along the bonding layer 10c in the hollow structure portion 10d formed in the ceramic sintered body portions 10a and 10b.
接合層１０ｃの厚さは、９μｍ〜２２５０μｍである。 The thickness of the bonding layer 10c is 9 μm to 2250 μm.
焼成前は、図１（ａ）及び図１（ｂ）を参照して、セラミックス成形体１１，１２の境界部分１１ｃ，１２ｃは、Ｃ面取りがなされている。そして、この面取り部は、焼成によって、接合面１０ｆ側の面取りされた部分の長さ（水平方向の面取り長さ）（図２（ａ）のＬ１参照）は０．０９ｍｍ〜４．５０ｍｍとなっている。また、面取り部の中空構造部１０ｄの内側面１０ｇ側の面取りされた部分の長さ（垂直方向の面取り長さ）（（図２（ａ）のＬ２参照）も０．０９ｍｍ〜４．５０ｍｍとなっている。 Before firing, referring to FIGS. 1A and 1B, the boundary portions 11c and 12c of the ceramic molded bodies 11 and 12 are chamfered. And this chamfered portion is 0.09 mm to 4.50 mm in length (horizontal chamfered length) (refer to L1 in FIG. 2A) of the chamfered portion on the joining surface 10f side by firing. ing. Further, the length of the chamfered portion of the hollow structure portion 10d of the chamfered portion on the inner surface 10g side (vertical chamfer length) (see L2 in FIG. 2A) is also 0.09 mm to 4.50 mm. It has become.
そして、この面取りされた部分の上に接合剤１３が染み出して、セラミックス焼結体部１０ａ，１０ｂに形成された中空構造部１０ｄに接合層１０ｃに沿って凹部１０ｅが形成されている。 The bonding agent 13 oozes out on the chamfered portion, and a recess 10e is formed along the bonding layer 10c in the hollow structure portion 10d formed in the ceramic sintered body portions 10a and 10b.
この凹部１０ｅ、接合剤１３の染み出し量に応じて相違する。接合剤１３の染み出しが少ないときには、図３（ａ）又は図３（ｂ）に示すように、接合層１０ｃの盛り上がりを中心に上下に２本並行に形成される。このとき、セラミックス焼結体部１０ａ，１０ｂの両方の面取り部の中空構造部１０ｄの内側面１０ｇ側の端部が露出している。 It differs depending on the amount of the recessed portion 10e and the bonding agent 13 that oozes out. When there is little seepage of the bonding agent 13, two are formed in parallel up and down around the rising of the bonding layer 10c as shown in FIG. 3 (a) or 3 (b). At this time, the edge part by the side of the inner surface 10g of the hollow structure part 10d of the chamfered part of both ceramic sintered compact parts 10a and 10b is exposed.
一方、接合剤１３の染み出しが多いときには、図３（ｃ）に示すように、接合層１０ｃが下方の面取り部の全面を覆い、凹部１０ｅは１本だけ形成される。このとき、セラミックス焼結体部１０ａのみ、面取り部の中空構造部１０ｄの内側面１０ｇ側の端部が露出している。 On the other hand, when the bonding agent 13 oozes out, as shown in FIG. 3C, the bonding layer 10c covers the entire surface of the lower chamfered portion, and only one recess 10e is formed. At this time, the edge part by the side of the inner surface 10g of the hollow structure part 10d of a chamfering part is exposed only for the ceramic sintered body part 10a.
焼成前に、図１（ｃ）を参照して、セラミックス焼結体部１０ａ，１０ｂの接合面１０ｆと中空構造部１０ｄとの境界部分にＲ面取りがなされている場合、接合剤１３の染み出しが少ないときには、例えば図３（ｄ）に示すように、接合層１０ｃの盛り上がりを中心に上下に凹部１０ｅは２本並行に形成される。一方、接合剤１３の染み出しが多いときには、凹部１０ｅは１本だけ形成され、セラミックス焼結体部１０ａのみ、面取り部の中空構造部１０ｄの内側面１０ｇ側の端部が露出する。 Before firing, referring to FIG. 1 (c), in the case where R chamfering is performed at the boundary between the joint surface 10f of the ceramic sintered body portions 10a and 10b and the hollow structure portion 10d, the bonding agent 13 oozes out. When there is little, for example, as shown in FIG. 3D, two concave portions 10e are formed in parallel up and down around the rising of the bonding layer 10c. On the other hand, when there is a large amount of seepage of the bonding agent 13, only one recess 10e is formed, and only the ceramic sintered body portion 10a is exposed at the end on the inner side surface 10g side of the hollow structure portion 10d of the chamfered portion.
焼成後は、図３（ａ）を参照して、中空構造部１０ｄの内側面１０ｇの表面粗さはＲａ１．２μｍ以下である。また、中空構造部１０ｄの縦断面において、鋭角、鈍角など角度に関係なく隅部１０ｈは、隅Ｒが０．０９ｍｍ〜４５．００ｍｍのＲ隅となっている。 After firing, referring to FIG. 3 (a), the surface roughness of the inner surface 10g of the hollow structure portion 10d is Ra 1.2 μm or less. Further, in the longitudinal section of the hollow structure portion 10d, the corner portion 10h has an R corner with a corner R of 0.09 mm to 45.00 mm regardless of an angle such as an acute angle or an obtuse angle.
（実施例及び比較例）
原料粉末として、Ａｌ２Ｏ３粉末１００質量部（昭和電工株式会社製／ＡＬ−１６０ＳＧ−３）に対して、バインダーとして、バインドセラム（三井東圧化学株式会社製／ＷＡ−３２０）を７．０質量部（外比）、分散剤として、アクリル酸系分散剤（東亞合成株式会社製／Ａ−６１１４）を２．０質量部（外比）が添加された水を溶媒としたスラリーを用意した。このスラリーを真空や加圧力を付与した鋳込み成形されることによって、直径５００ｍｍ、高さ６０ｍｍの円柱形状のセラミックス成形体１１，１２がそれぞれ作製された。
(Examples and Comparative Examples)
6. Bind serum (Mitsui Toatsu Chemical Co., Ltd./WA-320) is used as a binder for 100 parts by mass of Al 2 O 3 powder (manufactured by Showa Denko Co., Ltd./AL-160SG-3) as a raw material powder. Prepare slurry using 0 parts by mass (outer ratio) as a solvent and water with 2.0 parts by mass (outer ratio) of acrylic dispersant (Toagosei Co., Ltd./A-6114) added. did. Cylinder-shaped ceramic molded bodies 11 and 12 having a diameter of 500 mm and a height of 60 mm were produced by casting the slurry by applying a vacuum and a pressing force, respectively.
これらセラミックス成形体１１，１２の接合面１１ａ，１２ａに対してそれぞれ幅３０ｍｍ、深さ１５ｍｍの溝１１ｂ，１２ｂを渦巻き状となる形状に形成された。接合面１１ａ，１２ａと溝１１ｂ，１２ｂとの全ての境界部分に面取り長さが表１に記載の長さまでＣ面取り又はＲ面取りが施された。 Grooves 11b and 12b each having a width of 30 mm and a depth of 15 mm were formed in a spiral shape with respect to the joining surfaces 11a and 12a of the ceramic molded bodies 11 and 12, respectively. C-chamfering or R-chamfering was applied to all the boundary portions between the joining surfaces 11a and 12a and the grooves 11b and 12b until the chamfering length was as shown in Table 1.
さらに、溝１１ｂ，１２ｂの内側面１１ｄ，１２ｄを表面粗さが表１に記載の表面粗さになるまで研磨された。そして、溝１１ｂ，１２ｂの隅部１１ｅ，１２ｅは、比較例４のみを除き、Ｒ隅となるように加工された。
また、接合面１１ａ，１２ａを表面粗さが１．２μｍとなるまで研磨された。
Further, the inner surfaces 11d and 12d of the grooves 11b and 12b were polished until the surface roughness became the surface roughness shown in Table 1. Then, the corners 11e and 12e of the grooves 11b and 12b were processed so as to be R corners except for the comparative example 4.
Further, the bonding surfaces 11a and 12a were polished until the surface roughness became 1.2 μm.
さらに、実施例１，２，５及び比較例１，２，４，５では、接合剤１３として、表１に記載したように鋳込み成形で使用したスラリーと同配合のスラリーを用意した。実施例１及び比較例１では、このスラリー状の接合剤１３中に予め水中で含水させておいた成形体を浸漬させて、表１に記載の荷重を印加しながら、セラミックス成形体１１，１２の接合面１１ａ，１２ａにそれぞれ塗布された。 Furthermore, in Examples 1, 2, and 5 and Comparative Examples 1, 2, 4, and 5, as the bonding agent 13, as shown in Table 1, a slurry having the same composition as the slurry used in casting was prepared. In Example 1 and Comparative Example 1, the formed ceramics 11 and 12 were immersed in the slurry-like bonding agent 13 and immersed in water in advance, and the load shown in Table 1 was applied. Were applied to the joint surfaces 11a and 12a.
また、実施例２及び比較例５では、スラリー状の接合剤１３をセラミックス成形体１１，１２の接合面１１ａ，１２ａにそれぞれ刷毛で塗布した後、表１に記載の荷重を印加した。実施例５及び比較例２，４では、スラリー状の接合剤１３をセラミックス成形体１１，１２の接合面１１ａ，１２ａにそれぞれスプレーで噴霧した後、表１に記載の荷重を印加した。 In Example 2 and Comparative Example 5, the slurry-like bonding agent 13 was applied to the bonding surfaces 11a and 12a of the ceramic molded bodies 11 and 12 with a brush, and then the load shown in Table 1 was applied. In Example 5 and Comparative Examples 2 and 4, the slurry-like bonding agent 13 was sprayed on the bonding surfaces 11a and 12a of the ceramic molded bodies 11 and 12, respectively, and then the load shown in Table 1 was applied.
実施例３，６及び比較例３では、接合剤１３として、Ａｌ２Ｏ３粉末１００質量部（昭和電工株式会社製／ＡＬ−１６０ＳＧ−３）に対して、エチルセルロース系バインダーを５０．０質量部（外比）、フタル酸ジブチル系可塑剤を１６．７質量部（外比）が添加されたエチレングリコール、α−テルピネオール、エタノールなどの有機溶剤を溶媒としたペーストを用意した。 In Examples 3 and 6 and Comparative Example 3, as the bonding agent 13, 50.0 parts by mass of an ethyl cellulose binder with respect to 100 parts by mass of Al 2 O 3 powder (manufactured by Showa Denko KK / AL-160SG-3). (External ratio), a paste was prepared using an organic solvent such as ethylene glycol, α-terpineol, and ethanol, to which 16.7 parts by mass (external ratio) of dibutyl phthalate plasticizer was added.
そして、このペースト状の接合剤１３を、実施例３では印刷によって、実施例６及び比較例３では刷毛によって、セラミックス成形体１１，１２の接合面１１ａ，１２ａにそれぞれ塗布した後、表１に記載の荷重を印加した。 The paste-like bonding agent 13 was applied to the bonding surfaces 11a and 12a of the ceramic molded bodies 11 and 12 by printing in Example 3 and by brush in Example 6 and Comparative Example 3, respectively. The indicated load was applied.
実施例４では、接合剤１３として、Ａｌ２Ｏ３粉末１００質量部（昭和電工株式会社製／ＡＬ−１６０ＳＧ−３）に対して、エチルセルロース系バインダーを１３．０質量部（外比）、フタル酸ジブチル系可塑剤を１３．０質量部（外比）が添加されて作製されたエチレングリコール、α−テルピネオール、エタノールなどの有機溶剤を溶媒としたグリーンシートを用意した。 In Example 4, 13.0 parts by mass (external ratio) of ethyl cellulose binder is used as the bonding agent 13 with respect to 100 parts by mass of Al 2 O 3 powder (manufactured by Showa Denko KK / AL-160SG-3), phthalate A green sheet prepared by adding 13.0 parts by mass (external ratio) of a dibutyl acid plasticizer and using an organic solvent such as ethylene glycol, α-terpineol, and ethanol as a solvent was prepared.
そして、シート状の接合剤１３を、セラミックス成形体１１，１２の接合面１１ａ，１２ａにそれぞれ接合した後、表１に記載の荷重を印加した。 And after bonding the sheet-like bonding agent 13 to the bonding surfaces 11a and 12a of the ceramic molded bodies 11 and 12, respectively, the load shown in Table 1 was applied.
そして、実施例６では、接合剤１３を塗布した接合面１１ａ，１２ａを合わせた状態で、セラミックス成形体１１，１２をチャンバの内部に設置された。これらセラミックス成形体１１，１２に対して、等方的に静水圧プレスにより表１に記載の圧力が印加された。 In Example 6, the ceramic molded bodies 11 and 12 were placed inside the chamber in a state where the bonding surfaces 11a and 12a coated with the bonding agent 13 were combined. The pressures shown in Table 1 were applied isotropically to these ceramic compacts 11 and 12 by isostatic pressing.
成形体を十分に乾燥させた後、大気雰囲気中で１６００℃で３時間にわたり熱処理された。その結果、中空構造体１０が作製された（図３（ａ）参照）。 After the molded body was sufficiently dried, it was heat-treated at 1600 ° C. for 3 hours in an air atmosphere. As a result, the hollow structure 10 was produced (see FIG. 3A).
そして、中空構造体１０から、接合強度試験用の試験片が、接合層が中心にくるよう３ｍｍ×４ｍｍ×４０ｍｍの形状で切り出され、下部スパン３０ｍｍ、上部スパン１０ｍｍの４点曲げ試験によって接合強度が測定された（ＪＩＳＲ１６２４準拠）。 Then, a test piece for bonding strength test is cut out from the hollow structure 10 in a shape of 3 mm × 4 mm × 40 mm so that the bonding layer is at the center, and the bonding strength is obtained by a four-point bending test with a lower span of 30 mm and an upper span of 10 mm. Was measured (JISR1624 compliant).
表１には、各実施例及び各比較例の接合体の作製条件及び評価試験結果がまとめて示されている。 Table 1 summarizes the production conditions and evaluation test results of the joined bodies of the examples and the comparative examples.
（実施例１）
実施例１では、中空構造体１０の凹部１０ｅは、Ｒ面加工された固着物のない平滑な状態であった。そして、接合強度は３５０ＭＰａであり、母材強度の０．９５倍であって、気密性良好な接合状態であった。
Example 1
In Example 1, the concave portion 10e of the hollow structure 10 was in a smooth state with no R-face processed fixed matter. The bonding strength was 350 MPa, 0.95 times the strength of the base material, and a bonding state with good airtightness.
（実施例２）
実施例２では、中空構造体１０の凹部１０ｅは、実施例１同様であった。そして、接合強度は３２０ＭＰａであり、母材強度の０．８６倍であって、良好であった。
(Example 2)
In Example 2, the recess 10e of the hollow structure 10 was the same as that of Example 1. The bonding strength was 320 MPa, which was 0.86 times the base material strength and was good.
（実施例３〜５）
中空構造体１０の凹部１０ｅは実施例１，２と同様であり、接合強度も良好であった。
(Examples 3 to 5)
The recess 10e of the hollow structure 10 was the same as in Examples 1 and 2, and the bonding strength was good.
（実施例６）
実施例６では、接合後に１２００ｋｇｆ／ｃｍ２の圧力を印加してＣＩＰ成形を行った。中空構造体１０の凹部１０ｅは実施例１〜５と同様であり、接合強度も良好であった。
(Example 6)
In Example 6, CIP molding was performed by applying a pressure of 1200 kgf / cm 2 after joining. The recess 10e of the hollow structure 10 was the same as in Examples 1 to 5, and the bonding strength was also good.
（比較例１）
比較例１では、接合面と溝の交点における箇所に面取り加工を施さなかった。その箇所を基点としたクラックが発生した。
(Comparative Example 1)
In Comparative Example 1, chamfering was not performed at the intersection point between the joint surface and the groove. Cracks based on that location occurred.
（比較例２）
比較例２では、中空構造体１０の凹部１０ｅは、Ｒ面加工された固着物のない平滑な状態であった。そして、接合強度は１４０ＭＰａであり、母材強度の０．３８倍しかなく劣っていた。これは、面取り長さＬ１が０．０５ｍｍと０．１０ｍｍ未満であったため、接合剤１３の染み出しにより所定量の接合剤が不足したためである。
(Comparative Example 2)
In Comparative Example 2, the recess 10e of the hollow structure 10 was in a smooth state with no R-face processed fixed matter. The joint strength was 140 MPa, which was only 0.38 times the base material strength, and was inferior. This is because the chamfering length L1 was 0.05 mm and less than 0.10 mm, and the predetermined amount of the bonding agent was insufficient due to the bleeding of the bonding agent 13.
（比較例３）
比較例３では、接合強度は２９０ＭＰａであり、母材強度の０．７８倍であって、良好であった。しかし、中空構造部１０ｄの内側面１０ｇに接合剤１３が固着したものが見出された、これは、内側面１１ｄ、１２ｄの表面粗さが２．８μｍであり、２．０μｍを超えていたため、染み出した接合剤１３が固着したためである。
(Comparative Example 3)
In Comparative Example 3, the bonding strength was 290 MPa, which was 0.78 times the base material strength and was good. However, it was found that the bonding agent 13 was fixed to the inner side surface 10g of the hollow structural portion 10d, because the surface roughness of the inner side surfaces 11d and 12d was 2.8 μm and exceeded 2.0 μm. This is because the exuding bonding agent 13 is fixed.
（比較例４）
比較例４では、中空構造体１０の中空構造部１０ｄの隅部１０ｈを起点としたクラックが発生した。これは、セラミックス成形体１１，１２のそれぞれ溝１１ｂ，１２ｂの隅部１１ｅ，１２ｅはＲ隅に加工されておらず、角張った形状であったためである。
(Comparative Example 4)
In Comparative Example 4, a crack was generated starting from the corner 10h of the hollow structure 10d of the hollow structure 10. This is because the corners 11e and 12e of the grooves 11b and 12b of the ceramic molded bodies 11 and 12, respectively, are not machined into the R corner and have an angular shape.
（比較例５）
比較例５では、中空構造体１０の凹部１０ｅは、Ｒ面加工された固着物のない平滑な状態であった。そして、接合強度は１６０ＭＰａであり、母材強度の０．４３倍しかなく劣っていた。これは、面取り長さＬ１が７．００ｍｍと５．００ｍｍを超えていたため、スラリーの染み出しが多くなったためである。
(Comparative Example 5)
In Comparative Example 5, the concave portion 10e of the hollow structure 10 was in a smooth state with no R-face processed fixed matter. The bonding strength was 160 MPa, which was only 0.43 times the base material strength, and was inferior. This is because the chamfering length L1 exceeds 7.00 mm and 5.00 mm, so that the slurry exudes more.
１０…中空構造体、 １０ａ，１０ｂ…セラミックス焼結体部、 １０ｃ…接合層、 １０ｄ…中空構造部、 １０ｅ…凹部、 １０ｆ…接合面、 １０ｇ…中空構造部の内側面、 １０ｈ…中空構造部の隅部、 １１…第１のセラミックス成形体、 １２…第２のセラミックス成形体、 １１ａ，１２ａ…接合面、 １１ｂ，１２ｂ…溝、中空構造部となる部分、 １１ｃ，１２ｃ…境界部分、 １１ｄ，１２ｄ…溝の内側面、 １１ｅ，１２ｅ…溝の隅部、１３…接合剤。 DESCRIPTION OF SYMBOLS 10 ... Hollow structure, 10a, 10b ... Ceramic sintered body part, 10c ... Joining layer, 10d ... Hollow structure part, 10e ... Recessed part, 10f ... Joining surface, 10g ... Inner side surface of hollow structure part, 10h ... Hollow structure part 11 ... 1st ceramic molded body, 12 ... 2nd ceramic molded body, 11a, 12a ... Joining surface, 11b, 12b ... Groove, part which becomes a hollow structure part, 11c, 12c ... Boundary part, 11d , 12d: inner surface of the groove, 11e, 12e: corner of the groove, 13: bonding agent.
Claims (1)
前記セラミックス成形体の溝の内面を表面粗さＲａ２．０μｍ以下に加工する工程と、
前記セラミックス成形体と別のセラミックス成形体とを接合面に接合剤を介した状態で接合する工程と、
前記溝の底面部分だけを溶媒で洗浄する工程と、
前記接合したセラミックス成形体を焼成する工程とを備えることを特徴とする中空構造体の製造方法。 A ceramic molded body having a chamfered length of 0.10 mm to 5.00 mm is prepared at a boundary portion between the groove and the joint surface. And a process of
Processing the inner surface of the groove of the ceramic molded body to a surface roughness Ra of 2.0 μm or less;
Bonding the ceramic molded body and another ceramic molded body to a bonding surface through a bonding agent;
Washing only the bottom portion of the groove with a solvent;
And a step of firing the joined ceramic molded body.
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