JP2009078943A - Method for joining silicon carbide ceramic material - Google Patents
Method for joining silicon carbide ceramic material Download PDFInfo
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- JP2009078943A JP2009078943A JP2007248774A JP2007248774A JP2009078943A JP 2009078943 A JP2009078943 A JP 2009078943A JP 2007248774 A JP2007248774 A JP 2007248774A JP 2007248774 A JP2007248774 A JP 2007248774A JP 2009078943 A JP2009078943 A JP 2009078943A
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- silicon carbide
- carbide ceramic
- oxide film
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 39
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000005304 joining Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000005219 brazing Methods 0.000 claims abstract description 22
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 230000000873 masking effect Effects 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 16
- 239000011148 porous material Substances 0.000 abstract description 14
- 239000000945 filler Substances 0.000 abstract 2
- 239000002184 metal Substances 0.000 abstract 2
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- 239000006072 paste Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012993 chemical processing Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
Description
本発明は、炭化ケイ素セラミックス材同士をロウ材を介して接合する方法に関する。 The present invention relates to a method for joining silicon carbide ceramic materials together through a brazing material.
炭化ケイ素セラミックスは、耐熱性、耐熱衝撃性、耐食性等に優れ、高硬度であるという特徴を有しており、そのため、半導体製造装置用部材等に多用されている。
このような炭化ケイ素セラミックス部材は、用途によっては、各部材同士を接合して用いられる場合もある。
Silicon carbide ceramics are characterized by excellent heat resistance, thermal shock resistance, corrosion resistance, and the like, and high hardness. For this reason, silicon carbide ceramics are frequently used as members for semiconductor manufacturing equipment.
Such a silicon carbide ceramic member may be used by bonding each member depending on the application.
従来、前記炭化ケイ素セラミックス材同士の接合は、両者の接合面間に、粒状、ペースト状または粉末状等のシリコンや銀ロウ等からなる接合材を介して、該接合材の融点以上の温度で熱処理することにより行われていた（例えば、特許文献１，２参照）。
しかしながら、炭化ケイ素セラミックス材を細孔や溝等を有する面で接合させる場合は、上記のような従来の接合方法では、前記細孔や溝等の微細空間が、溶融したシリコンや銀ロウ等の侵入によって閉塞するため、このような細孔や溝等を維持した状態の接合体を得ることが困難であった。 However, when the silicon carbide ceramic material is bonded on the surface having pores, grooves, etc., in the conventional bonding method as described above, the fine spaces such as the pores, grooves, etc. Since it is blocked by intrusion, it is difficult to obtain a bonded body in a state in which such pores and grooves are maintained.
本発明は、上記技術的課題を解決するためになされたものであり、細孔や溝等を有する複雑な形状の炭化ケイ素セラミックス材であっても、前記細孔や溝等を接合材により閉塞させることなく、接合体を得ることができる炭化ケイ素セラミックス材の接合方法を提供することを目的とするものである。 The present invention has been made to solve the above technical problem, and even in the case of a silicon carbide ceramic material having a complicated shape having pores and grooves, the pores and grooves are blocked with a bonding material. An object of the present invention is to provide a method for joining silicon carbide ceramic materials, which can obtain a joined body without causing the joining.
本発明に係る炭化ケイ素セラミックス材の接合方法は、炭化ケイ素セラミックス材同士を、シリコンを含むロウ材を用いて接合させる際、前記炭化ケイ素セラミックス材の非接合面に、予め、酸化膜を形成しておくことを特徴とする。
上記接合方法によれば、細孔や溝等を有する複雑な形状の炭化ケイ素セラミックス材であっても、非接合面を酸化膜で被覆する工程を経るのみで、形成前記細孔や溝等をロウ材による接合材により閉塞することのない接合体を簡便に得ることができる。
In the method for bonding silicon carbide ceramic materials according to the present invention, when silicon carbide ceramic materials are bonded to each other using a brazing material containing silicon, an oxide film is formed in advance on the non-bonded surface of the silicon carbide ceramic material. It is characterized by keeping.
According to the above bonding method, even if it is a silicon carbide ceramic material having a complicated shape having pores, grooves, etc., the formation of the pores, grooves, etc. can be performed only by undergoing a process of coating the non-bonded surface with an oxide film. A joined body that is not blocked by the joining material of the brazing material can be easily obtained.
上記接合方法において、前記酸化膜は、炭化ケイ素セラミックス材の表面よりもロウ材が付着しにくい、すなわち、炭化ケイ素セラミックス材表面よりも濡れにくい、干渉色を示すような酸化膜として形成させるため、接合面をマスキングし、ＣＶＤ法により、非接合面にのみ形成することが好ましい。
あるいはまた、熱酸化法、ＣＶＤ法またはプラズマ酸化法により、炭化ケイ素セラミックス材全体に酸化膜を形成した後、接合面の酸化膜のみ、研削またはエッチングにより除去して形成してもよい。
In the above bonding method, the oxide film is less likely to adhere to the brazing material than the surface of the silicon carbide ceramic material, that is, less likely to wet than the silicon carbide ceramic material surface, so as to form an oxide film that exhibits an interference color. It is preferable that the bonding surface is masked and formed only on the non-bonding surface by a CVD method.
Alternatively, after forming an oxide film on the entire silicon carbide ceramic material by a thermal oxidation method, a CVD method or a plasma oxidation method, only the oxide film on the bonding surface may be removed by grinding or etching.
上述したとおり、本発明に係る炭化ケイ素セラミックス材の接合方法によれば、細孔や溝等を有する複雑な形状の炭化ケイ素セラミックス材であっても、前記細孔や溝等を接合材により閉塞させることなく、接合体を得ることができる。
したがって、本発明に係る接合方法は、細孔や溝等を有するような接合面形状が複雑な定盤やエッチャー用チャンバ、真空チャック、ラッププレート等の半導体製造装置用部材の製造にも好適に適用することができる。
As described above, according to the silicon carbide ceramic material joining method according to the present invention, even if the silicon carbide ceramic material has a complicated shape having pores, grooves, etc., the pores, grooves, etc. are blocked by the joining material. A joined body can be obtained without causing them to occur.
Therefore, the bonding method according to the present invention is also suitable for manufacturing a member for a semiconductor manufacturing apparatus such as a surface plate, an etcher chamber, a vacuum chuck, or a lap plate having a complicated bonding surface shape having pores, grooves, and the like. Can be applied.
以下、本発明について、より詳細に説明する。
本発明に係る炭化ケイ素セラミックス材の接合方法は、炭化ケイ素セラミックス材同士を、シリコンを含むロウ材を用いて接合させる際、前記炭化ケイ素セラミックス材の非接合面に、予め、酸化膜を形成しておくことを特徴とするものである。
すなわち、本発明に係る接合方法においては、炭化ケイ素セラミックス材の表面のうち、ロウ材を付着させたくない面を、予め、酸化膜で被膜された状態としておく。
酸化膜で被覆された面と、被覆されていない、炭化ケイ素セラミックスの露出面とでは、ロウ材のぬれ性が異なり、そのぬれ性は、炭化ケイ素よりも、酸化ケイ素の方が低い。
このため、酸化膜表面はロウ材が付着しにくくなり、接合させようとする面にのみロウ材を介在させて、接合させることができる。
Hereinafter, the present invention will be described in more detail.
In the method for bonding silicon carbide ceramic materials according to the present invention, when silicon carbide ceramic materials are bonded to each other using a brazing material containing silicon, an oxide film is formed in advance on the non-bonded surface of the silicon carbide ceramic material. It is characterized by keeping.
That is, in the bonding method according to the present invention, the surface of the silicon carbide ceramic material on which the brazing material is not desired to be deposited is previously coated with an oxide film.
The wettability of the brazing material is different between the surface covered with the oxide film and the exposed surface of the silicon carbide ceramic that is not covered, and the wettability of silicon oxide is lower than that of silicon carbide.
For this reason, it becomes difficult for the brazing material to adhere to the surface of the oxide film, and the brazing material can be interposed and bonded only to the surfaces to be joined.
したがって、例えば、定盤やエッチャー用チャンバ、真空チャック、ラッププレート等の半導体製造装置用部材の製造において、細孔や溝等を有する複雑な形状の炭化ケイ素セラミックス材を接合させる場合であっても、非接合面を酸化膜で被覆する工程を経るのみで、前記細孔や溝等をロウ材による接合材により閉塞することのない接合体を簡便に得ることができる。 Therefore, for example, in the manufacture of a semiconductor manufacturing apparatus member such as a surface plate, an etcher chamber, a vacuum chuck, or a lap plate, even when a silicon carbide ceramic material having a complicated shape having pores or grooves is joined. In addition, it is possible to easily obtain a joined body in which the pores, the grooves and the like are not blocked by the joining material made of the brazing material only through the process of covering the non-joined surface with the oxide film.
前記酸化膜は、上記のように、ロウ材を付着しにくくさせるためには、自然酸化膜ではなく、干渉色を示すような酸化膜とする必要がある。
具体的には、前記酸化膜は、熱酸化法、ＣＶＤ法、プラズマ酸化法等により形成することが好ましい。また、前記酸化膜の厚さは、１０ｎｍ以上２５０ｎｍ以下であることが好ましい。
As described above, in order to make the brazing material difficult to adhere, the oxide film needs to be an oxide film that exhibits an interference color, not a natural oxide film.
Specifically, the oxide film is preferably formed by a thermal oxidation method, a CVD method, a plasma oxidation method, or the like. The thickness of the oxide film is preferably 10 nm or more and 250 nm or less.
上記のような酸化膜を非接合面にのみ形成する方法としては、例えば、ロウ材を付着させようとする接合面をマスキングして、ＣＶＤ法等により、非接合面に酸化膜を形成する方法を用いることができる。
あるいはまた、熱酸化法、ＣＶＤ法またはプラズマ酸化法等により、炭化ケイ素セラミックス材全体に酸化膜を形成した後、平面研削盤やサンドブラストによる機械的加工、または、アルカリ薬液等によるエッチング等の化学的処理により、接合面の酸化膜のみを除去する方法も用いることができる。
As a method of forming the oxide film as described above only on the non-joint surface, for example, a method of forming the oxide film on the non-joint surface by CVD or the like by masking the joint surface to which the brazing material is to be attached Can be used.
Alternatively, after an oxide film is formed on the entire silicon carbide ceramic material by a thermal oxidation method, a CVD method, a plasma oxidation method, etc., chemical processing such as mechanical processing by a surface grinder or sandblast, or etching by an alkaline chemical solution, etc. A method of removing only the oxide film on the bonding surface by the treatment can also be used.
本発明において用いられる接合材であるロウ材は、特に制限されるものではなく、従来から炭化ケイ素セラミックス材の接合に用いられているシリコンを含むロウ材（例えば、アルミシリコンやシリコン等）を使用することができる。また、ロウ材の形状も、特に限定されるものではなく、粒状、ペースト状、板状等のいずれであってもよい。
上記のようなロウ材を、炭化ケイ素セラミックス材の接合面間に挟み込み、所定温度で熱処理することにより、前記ロウ材が溶融して流れ込み、接合面同士が接合される。
The brazing material that is a bonding material used in the present invention is not particularly limited, and a brazing material containing silicon (for example, aluminum silicon or silicon) that has been conventionally used for bonding silicon carbide ceramic materials is used. can do. Further, the shape of the brazing material is not particularly limited, and may be any of a granular shape, a paste shape, a plate shape, and the like.
The brazing material as described above is sandwiched between the joining surfaces of the silicon carbide ceramic material and heat treated at a predetermined temperature, whereby the brazing material melts and flows, and the joining surfaces are joined.
以下、本発明を実施例に基づきさらに具体的に説明するが、本発明は下記の実施例により制限されるものではない。
［実施例１］
５０ｍｍ×５０ｍｍ×厚さ１０ｍｍの常圧焼結炭化ケイ素セラミックス材に、幅２ｍｍ、深さ２．５ｍｍの溝１を３本形成し、図１に示すような形状の試料片を作製した。
この試料片を熱酸化処理し、全面に厚さ２００〜２５０ｎｍの酸化膜を形成した。
そして、接合面２（図１の試料片の上面）を、平面研削盤で表面から厚さ０．５ｍｍ研削した。
この試料片２枚を、接合面間に、ペースト状のシリコン（純度９９％以上）を介在させて、０．０１Ｔｏｒｒの真空雰囲気中、１５００℃で０．５時間熱処理し、図２に示すような接合体を作製した。
上記のような接合体を５０個作製し、それぞれについて、超音波画像装置により、シリコン（ロウ材）による溝の閉塞の有無を調べた結果、接合体５０個のうち、溝がシリコンにより閉塞しているものは認めらなかった。
EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Example 1]
Three
This sample piece was thermally oxidized to form an oxide film having a thickness of 200 to 250 nm on the entire surface.
And the joining surface 2 (upper surface of the sample piece of FIG. 1) was ground 0.5 mm in thickness from the surface with the surface grinder.
Two sample pieces were heat-treated at 1500 ° C. for 0.5 hours in a vacuum atmosphere of 0.01 Torr with paste-like silicon (purity 99% or more) interposed between the joining surfaces, as shown in FIG. A simple joined body was produced.
As a result of producing 50 bonded bodies as described above and checking the presence or absence of the clogging of the groove with silicon (brazing material) with an ultrasonic imaging apparatus, the groove was blocked with silicon in the 50 bonded bodies. We did not recognize what was.
［比較例１］
酸化処理を施さず、それ以外については、実施例１と同様にして、接合体を作製し、シリコンによる溝の閉塞の有無を調べた。
その結果、接合体５０個のうち１８個について、溝がシリコンにより閉塞していることが確認された。
[Comparative Example 1]
Other than that, a joined body was prepared in the same manner as in Example 1, and the presence or absence of the clogging of the groove with silicon was examined.
As a result, it was confirmed that the grooves of 18 of the 50 bonded bodies were closed with silicon.
［実施例２］
５０ｍｍ×５０ｍｍ×厚さ１０ｍｍの常圧焼結炭化ケイ素セラミックス材に、直径１ｍｍの貫通孔３を１０ｍｍ間隔で１６個形成し、図３に示すような形状の試料片を作製した。
この試料片を熱酸化処理し、全面に厚さ２００〜２５０ｎｍの酸化膜を形成した。
そして、接合面４（図３の試料片の上面）を、平面研削盤で表面から厚さ０．５ｍｍ研削した。
この試料片２枚を、接合面間に、ペースト状のシリコン（純度９９％以上）を介在させて、０．０１Ｔｏｒｒの真空雰囲気中、１５００℃で０．５時間熱処理し、図４に示すような接合体を作製した。
上記のような接合体を５０個作製し、それぞれについて、超音波画像装置により、シリコン（ロウ材）による孔の閉塞の有無を調べた結果、接合体５０個のうち、孔がシリコンにより閉塞しているものは認めらなかった。
[Example 2]
Sixteen through-
This sample piece was thermally oxidized to form an oxide film having a thickness of 200 to 250 nm on the entire surface.
And the joining surface 4 (upper surface of the sample piece of FIG. 3) was ground 0.5 mm in thickness from the surface with the surface grinder.
The two sample pieces were heat-treated at 1500 ° C. for 0.5 hours in a 0.01 Torr vacuum atmosphere with paste-like silicon (purity 99% or more) interposed between the joining surfaces, as shown in FIG. A simple joined body was produced.
As a result of preparing 50 bonded bodies as described above and checking the presence or absence of holes blocked by silicon (brazing material) using an ultrasonic imaging apparatus, the holes of 50 bonded bodies were blocked by silicon. We did not recognize what was.
［比較例１］
酸化処理を施さず、それ以外については、実施例１と同様にして、接合体を作製し、シリコンによる孔の閉塞の有無を調べた。
その結果、接合体５０個のうち３０個について、孔がシリコンにより閉塞していることが確認された。
[Comparative Example 1]
Other than that, a joined body was prepared in the same manner as in Example 1, and the presence / absence of clogging of holes by silicon was examined.
As a result, it was confirmed that 30 holes out of 50 bonded bodies were closed with silicon.
１ 溝
２，４ 接合面
３ 孔
1
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019001695A (en) * | 2017-06-19 | 2019-01-10 | 日本特殊陶業株式会社 | Method for producing silicon carbide member |
| WO2022210470A1 (en) * | 2021-03-29 | 2022-10-06 | 京セラ株式会社 | Method for producing assembly |
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| JP2003192463A (en) * | 2001-12-26 | 2003-07-09 | Kyocera Corp | Nitride ceramic copper circuit board |
| JP2005289744A (en) * | 2004-03-31 | 2005-10-20 | Toshiba Corp | Method for manufacturing reaction sintered silicon carbide structure |
| JP2007153700A (en) * | 2005-12-07 | 2007-06-21 | Toshiba Ceramics Co Ltd | Method of joining silicon carbide porous ceramic and joined member |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003192463A (en) * | 2001-12-26 | 2003-07-09 | Kyocera Corp | Nitride ceramic copper circuit board |
| JP2005289744A (en) * | 2004-03-31 | 2005-10-20 | Toshiba Corp | Method for manufacturing reaction sintered silicon carbide structure |
| JP2007153700A (en) * | 2005-12-07 | 2007-06-21 | Toshiba Ceramics Co Ltd | Method of joining silicon carbide porous ceramic and joined member |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019001695A (en) * | 2017-06-19 | 2019-01-10 | 日本特殊陶業株式会社 | Method for producing silicon carbide member |
| WO2022210470A1 (en) * | 2021-03-29 | 2022-10-06 | 京セラ株式会社 | Method for producing assembly |
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| JP4954838B2 (en) | 2012-06-20 |
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