JP2002145677A - Jointed body of silicon carbide sintered compact, member for producing semiconductor using the same and method of producing the same - Google Patents

Jointed body of silicon carbide sintered compact, member for producing semiconductor using the same and method of producing the same

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Publication number
JP2002145677A
JP2002145677A JP2000341881A JP2000341881A JP2002145677A JP 2002145677 A JP2002145677 A JP 2002145677A JP 2000341881 A JP2000341881 A JP 2000341881A JP 2000341881 A JP2000341881 A JP 2000341881A JP 2002145677 A JP2002145677 A JP 2002145677A
Authority
JP
Japan
Prior art keywords
sintered
sic
same
producing
bonded
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP2000341881A
Other languages
Japanese (ja)
Inventor
Tatsuya Tsuyuki
龍也 露木
Shunichi Suzuki
俊一 鈴木
Masahiko Ichijima
雅彦 市島
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Coorstek KK
Original Assignee
Toshiba Ceramics Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Toshiba Ceramics Co Ltd filed Critical Toshiba Ceramics Co Ltd
Priority to JP2000341881A priority Critical patent/JP2002145677A/en
Publication of JP2002145677A publication Critical patent/JP2002145677A/en
Pending legal-status Critical Current

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  • Drying Of Semiconductors (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a jointed body of SiC sintered compacts being the jointed body whose jointing strength is always high. SOLUTION: SiC sintered compacts 1 and 2, each obtained by pressureless sintering and having a bulk density of >=2.8 g/cm3 are jointed to each other through a jointing part 3 comprising Si and filling parts 4 and 5 comprising Si which is filled in open pores 1a and 2a opening to the jointing face of the SiC sintered compacts and being unified with the Si at the jointing part 3.

Description

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

【0001】[0001]

【発明の属する技術分野】本発明は、SiC(炭化珪
素)焼結体(SiCセラミックス)の接合体、それを利
用した定盤、エッチャー用チャンバ等の半導体製造用部
材、及びその製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a joined body of sintered SiC (silicon carbide) (SiC ceramics), a member for producing a semiconductor such as a surface plate and an etcher chamber using the same, and a method of producing the same.

【0002】[0002]

【従来の技術】従来、この種のSiC焼結体の接合体と
しては、2〜40wt%のSiと60〜98wt%のSiC
を含有する反応焼結SiC焼結体同士がSiからなる接
合部を介して接合されているものが知られている(特開
平6−128046号公報)。上記SiC焼結体の接合
体は、反応焼結SiC焼結体同士の接合面にSi粉末を
塗布し、アルゴンガス雰囲気等の非酸化性雰囲気におい
て熱処理した後、室温まで徐冷して製造されるものであ
る。
2. Description of the Related Art Conventionally, as a bonded body of this type of SiC sintered body, 2 to 40 wt% of Si and 60 to 98 wt% of SiC have been used.
(Japanese Patent Application Laid-Open No. 6-128046) is known in which reaction-sintered SiC sintered bodies each containing Si are joined via a joint made of Si. The bonded body of the SiC sintered body is manufactured by applying Si powder to a bonding surface of the reaction sintered SiC sintered bodies, heat-treating the same in a non-oxidizing atmosphere such as an argon gas atmosphere, and then gradually cooling to room temperature. Things.

【0003】[0003]

【発明が解決しようとする課題】しかし、従来のSiC
焼結体の接合体及びその製造方法では、接合体の接合強
度が、表面粗さ等の接合面の表面状態により変化する不
具合がある。これは、接合面は、ある程度の精度が必要
であり、特に、接合面積が大きくなればなるほど、平坦
度が重要となるが、単純なSi接合であると、接合は接
合材であるSiとSiC焼結体の接合面との濡れによっ
て生じているため、接合面の加工精度を上げるとその表
面状態も変わるので、接合強度にばらつきを生じてしま
うからと考えられる。
However, the conventional SiC
In the joined body of the sintered body and the method of manufacturing the same, there is a problem that the joining strength of the joined body changes depending on the surface condition of the joining surface such as the surface roughness. This is because the bonding surface requires a certain degree of accuracy, and in particular, as the bonding area increases, the flatness becomes more important. However, in the case of a simple Si bonding, the bonding is performed using the bonding materials Si and SiC. It is considered that this is caused by wetting of the sintered body with the bonding surface, and if the processing accuracy of the bonding surface is increased, the surface state also changes, thereby causing variation in bonding strength.

【0004】そこで、本発明は、常に高接合強度の接合
体とし得るSiC焼結体の接合体、それを利用して半導
体製造用部材、及びその製造方法を提供することを目的
とする。
Accordingly, an object of the present invention is to provide a bonded body of a SiC sintered body which can always be a bonded body having a high bonding strength, a semiconductor manufacturing member using the same, and a manufacturing method thereof.

【0005】[0005]

【課題を解決するための手段】前記課題を解決するた
め、本発明のSiC焼結体の接合体は、嵩密度2.8g/
cm3 以上の常圧焼結SiC焼結体同士がSiからなる接
合部及び常圧焼結SiC焼結体の接合面に開口する開気
孔に充填されて接合部と一体のSiからなる充填部を介
して接合されていることを特徴とする。
Means for Solving the Problems In order to solve the above problems, the bonded body of the SiC sintered body of the present invention has a bulk density of 2.8 g /
A pressure-sintered SiC sintered body having a size of 3 cm or more is filled into a joint portion made of Si and an open pore opening in a joining surface of the pressure-sintered SiC sintered body, and a filling portion made of Si integrated with the joint portion Characterized by being joined via

【0006】半導体製造用部材は、上記SiC焼結体の
接合体を利用したことを特徴とする。
[0006] A member for manufacturing a semiconductor is characterized by utilizing a joined body of the above-described SiC sintered body.

【0007】一方、SiC焼結体の接合体の製造方法
は、嵩密度2.8g/cm3 以上の常圧焼結SiC焼結体の
接合面にSiを載せ、非酸化性雰囲気又は真空雰囲気に
おいてSiの融点以上の温度で熱処理した後、常圧焼結
SiC焼結体同士の接合面間にSiを介在し、非酸化性
雰囲気又は真空雰囲気においてSiの融点以上の温度で
熱処理することを特徴とする。上記Siは、板状、粒状
又は粉状であることが好ましい。
On the other hand, a method of manufacturing a bonded SiC sintered body is such that Si is placed on a bonded surface of a normal pressure sintered SiC sintered body having a bulk density of 2.8 g / cm 3 or more, and a non-oxidizing atmosphere or a vacuum atmosphere is used. After the heat treatment at a temperature equal to or higher than the melting point of Si, the heat treatment is performed at a temperature equal to or higher than the melting point of Si in a non-oxidizing atmosphere or a vacuum atmosphere by interposing Si between the bonding surfaces of the normal pressure sintered SiC sintered bodies. Features. The Si is preferably in the form of plate, granule or powder.

【0008】前記Si焼結体の接合体及びその製造方法
においては、接合材としてのSiが、接合面に開口する
開気孔に充填された充填材としてのSiによって足付き
効果(アンカー効果)を有するものとなる。
In the bonded body of the Si sintered body and the method of manufacturing the same, Si as a bonding material has a footing effect (anchor effect) due to Si as a filler filled in open pores opened on a bonding surface. Will have.

【0009】常圧焼結SiC焼結体の嵩密度2.8g/cm
3 未満であると、接合熱処理時に接合材としてのSi
が、接合面に開口する開気孔に充填された充填材として
のSiと共に常圧焼結SiC焼結体の気孔中に吸い込ま
れてしまい、接合が困難となる。常圧焼結SiC焼結体
の嵩密度は、3.0g/cm3 以上が好ましい。
The bulk density of the normal pressure sintered SiC sintered body is 2.8 g / cm.
If it is less than 3 , Si as a bonding material during the bonding heat treatment
Is sucked into the pores of the normal pressure sintered SiC sintered body together with the Si as the filler filled in the open pores opened to the joint surface, making the joining difficult. The bulk density of the normal pressure sintered SiC sintered body is preferably 3.0 g / cm 3 or more.

【0010】雰囲気を非酸化性又は真空とするのは、S
iの酸化を防止するためである。非酸化性雰囲気として
は、アルゴンガスや窒素ガス、ヘリウムガス等が用いら
れ、真空雰囲気としては0.01Torr以下の真空が用い
られる。
[0010] The atmosphere is made non-oxidizing or vacuum because S
This is to prevent oxidation of i. As the non-oxidizing atmosphere, an argon gas, a nitrogen gas, a helium gas or the like is used, and as the vacuum atmosphere, a vacuum of 0.01 Torr or less is used.

【0011】熱処理温度が、Siの融点未満であると、
Siが融解されず、接合面へ開口した開気孔への充填、
接合が困難となる。Siの融点以上の温度としては、1
450〜1600℃が好ましく、1480〜1500℃
がより好ましい。
When the heat treatment temperature is lower than the melting point of Si,
Filling of open pores opened to the joint surface without Si melting
Joining becomes difficult. The temperature above the melting point of Si is 1
450-1600 ° C is preferred, 1480-1500 ° C
Is more preferred.

【0012】板状のSiの厚みは、0.1〜0.5mmが
好ましくは、0.2〜0.3mmがより好ましい。粒状の
Siの粒径は、0.05〜0.2mmが好ましく、0.0
5〜0.1mmがより好ましい。又、粒状のSiは、エタ
ノールと混合してペースト状として用いる。粉状のSi
の粒径は、0.1〜10μmが好ましく、1〜5μmが
より好ましい。又、粉状のSiは、エタノールと混合し
てスラリー状として用いる。
The thickness of the plate-like Si is preferably 0.1 to 0.5 mm, more preferably 0.2 to 0.3 mm. The particle size of the granular Si is preferably 0.05 to 0.2 mm, and 0.0
More preferably, it is 5 to 0.1 mm. Granular Si is mixed with ethanol and used as a paste. Powdery Si
Is preferably from 0.1 to 10 μm, more preferably from 1 to 5 μm. The powdery Si is mixed with ethanol and used as a slurry.

【0013】又、前記半導体製造用部材においては、常
圧焼結SiC焼結体同士が足付き効果を有するSiから
なる充填材、接合材を介して接合された接合体を利用す
ることにより、充填材、接合材による不純物汚染が格段
に低減される。
In the above-mentioned semiconductor manufacturing member, a normal pressure sintered SiC sintered body is bonded to each other by using a filler and a bonding material made of Si having a footing effect. Impurity contamination by the filler and the bonding material is remarkably reduced.

【0014】Si以外の接合材を用いると、それ自体が
半導体製造プロセスにおいて不純物になること、接合の
際の熱処理時に、接合材が被接合材としての常圧焼結S
iC焼結体の組織内に不純物として拡散してしまうこと
により、接合体を実際に半導体製造プロセスにおいて使
用した場合、シリコンウェーハ等の半導体基板を汚染し
て歩留まりを低下させてしまう。
If a bonding material other than Si is used, the bonding material itself becomes an impurity in a semiconductor manufacturing process, and the bonding material becomes a normal pressure sintered S
By diffusing as an impurity into the structure of the iC sintered body, when the joined body is actually used in a semiconductor manufacturing process, a semiconductor substrate such as a silicon wafer is contaminated and the yield is reduced.

【0015】[0015]

【発明の実施の形態】以下、本発明の実施の形態につい
て具体的な実施例、比較例を参照して説明する。 実施例1〜3 先ず、嵩密度が2.8g/cm3 (実施例1)、2.9g/cm
3 (実施例2)、及び3.1g/cm3 の常圧焼結SiC焼
結体(100×200×20mm)の接合面上に、粒径
0.05mmの顆粒状のSiをエタノールと混合してペー
スト状としたものを塗布し、0.01Torrの真空雰囲気
において1500℃の温度で0.5時間熱処理した。熱
処理後における各常圧焼結SiC焼結体の接合面に開口
する開気孔には、Siが充填されていた。次に、嵩密度
が同じ常圧焼結SiC焼結体同士の接合面間に、厚み
0.02mmの板状のSiを介在し、0.01Torrの真空
雰囲気において1500℃の温度で0.5時間熱処理し
た後、室温まで徐冷して各常圧焼結SiC焼結体の接合
体を得た。
DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below with reference to specific examples and comparative examples. Examples 1 to 3 First, the bulk density was 2.8 g / cm 3 (Example 1), 2.9 g / cm 3
3 (Example 2) and 3.1 g / cm 3 of a normal pressure sintered SiC sintered body (100 × 200 × 20 mm), on which a granular Si having a particle diameter of 0.05 mm was mixed with ethanol. Then, a paste was applied and heat-treated at 1500 ° C. for 0.5 hour in a vacuum atmosphere of 0.01 Torr. After the heat treatment, Si was filled in the open pores opened on the joint surface of each normal pressure sintered SiC sintered body. Next, a plate-like Si having a thickness of 0.02 mm is interposed between bonding surfaces of the normal-pressure sintered SiC sintered bodies having the same bulk density, and 0.5 mm at a temperature of 1500 ° C. in a vacuum atmosphere of 0.01 Torr. After the heat treatment for an hour, the mixture was gradually cooled to room temperature to obtain a bonded body of each normal pressure sintered SiC sintered body.

【0016】得られた各常圧焼結体SiC焼結体の接合
体の接合4点曲げ強度(JIS−R1624)は、図1
に示すように、1000℃の温度で150MPa(実施
例1)、170MPa(実施例2)、及び200MPa
(実施例3)であった。又、各常圧焼結SiC焼結体の
接合体の断面を観たところ、図2に示すように、常圧焼
結SiC焼結体1,2同士が、Siからなる接合体3及
び常圧焼結SiC焼結体1,2の接合面に開口する開気
孔1a,2aに充填されて接合部3と一体のSiからな
る充填部4,5を介して接合されていた。
The joint four-point bending strength (JIS-R1624) of the obtained joint body of each normal pressure sintered body SiC sintered body is shown in FIG.
As shown in FIG. 5, 150 MPa (Example 1), 170 MPa (Example 2), and 200 MPa at a temperature of 1000 ° C.
(Example 3). Further, when the cross section of the joined body of each normal pressure sintered SiC sintered body was observed, as shown in FIG. Open holes 1a, 2a opened in the joint surfaces of the pressure-sintered SiC sintered bodies 1, 2 are filled and joined to the joint 3 via filling portions 4 and 5 made of Si.

【0017】比較例1〜3 嵩密度が、2.8g/cm3 (比較例1)、3.0g/cm3
(比較例2)、及び3.1g/cm3 (比較例3)の常圧焼
結体SiC焼結体(100×200×20mm)同士の接
合面間に、厚み0.02mmの板状のSiを介在し、0.
01Torrの真空雰囲気において1500℃の温度で0.
5時間熱処理した後、室温まで徐冷したところ、比較例
1のものは、Siが常圧焼結SiC焼結体の気孔中に吸
い込まれ、接合できなかったが、比較例2,3のもの
は、接合体が得られた。得られた比較例2,3の常圧焼
結SiC焼結体の接合体の接合4点曲げ強度(JISR
1624)は、1000℃の温度で150MPa(比較
例2)、160MPa(比較例3)であった。
Comparative Examples 1 to 3 The bulk density was 2.8 g / cm 3 (Comparative Example 1), 3.0 g / cm 3
(Comparative Example 2) and a normal pressure sintered body of 3.1 g / cm 3 (Comparative Example 3) A 0.02 mm-thick plate-like member is formed between joining surfaces of SiC sintered bodies (100 × 200 × 20 mm). With Si interposed, 0.
0.1 ° C. at a temperature of 1500 ° C. in a vacuum atmosphere of 01 Torr.
After the heat treatment for 5 hours, the temperature was gradually cooled to room temperature. In the case of Comparative Example 1, Si was sucked into the pores of the normal pressure sintered SiC sintered body and could not be joined. A conjugate was obtained. Four-point bending strength (JISR) of the obtained joints of the normal pressure sintered SiC sintered bodies of Comparative Examples 2 and 3
1624) were 150 MPa (Comparative Example 2) and 160 MPa (Comparative Example 3) at a temperature of 1000 ° C.

【0018】なお、上述した各実施例においては、顆粒
状や板状のSiを融解させる熱処理を真空雰囲気におい
て行う場合について説明したが、アルゴンガスや窒素ガ
ス等の非酸化性雰囲気で行っても同様の作用効果が得ら
れた。又、充填材、接合材としてのSiは、顆粒状や板
状のものに限らず、粉状のものとしても同様の作用効果
が得られた。
In each of the embodiments described above, the case where the heat treatment for melting the granular or plate-like Si is performed in a vacuum atmosphere is described, but the heat treatment may be performed in a non-oxidizing atmosphere such as argon gas or nitrogen gas. Similar effects were obtained. In addition, Si as a filler and a bonding material was not limited to a granular or plate-like material, and the same effect was obtained even when a powdery material was used.

【0019】一方、実施例1〜3と同様の常圧焼結Si
C焼結体の接合体を、半導体製造用部材としての定盤、
エッチャー用チャンバ等として用いたところ、それらに
よる半導体基板の汚染を格段に低減することができた。
On the other hand, the same normal pressure sintered Si as in Examples 1 to 3 was used.
A bonded body of the C sintered body is used as a surface plate as a semiconductor manufacturing member,
When used as an etcher chamber or the like, contamination of the semiconductor substrate by such chambers was significantly reduced.

【0020】[0020]

【発明の効果】以上説明したように、本発明のSiC焼
結体の接合体及びその製造方法によれば、接合材として
のSiが、接合面に開口する開気孔に充填された充填材
としてのSiによって足付き効果を有するものとなるの
で、従来のものに比べ、常に高接合強度のものとするこ
とができる。
As described above, according to the bonded SiC sintered body and the method of manufacturing the same according to the present invention, Si as a bonding material is used as a filler filled in open pores opened on a bonding surface. Since Si has a footing effect, it can always have a higher bonding strength than the conventional one.

【0021】一方、上記接合体を利用した半導体製造用
部材によれば、充填材、接合材による不純物の汚染が格
段に低減されるので、半導体基板の歩留まりを向上する
ことができる。
On the other hand, according to the semiconductor manufacturing member using the above-mentioned bonded body, contamination of impurities by the filler and the bonding material is remarkably reduced, so that the yield of the semiconductor substrate can be improved.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明に係るSiC焼結体の接合体における常
圧焼結SiC焼結体の嵩密度と接合体の接合強度の関係
を示す説明図である。
FIG. 1 is an explanatory diagram showing the relationship between the bulk density of a normal pressure sintered SiC sintered body and the joining strength of the joined body in the joined body of SiC sintered bodies according to the present invention.

【図2】本発明に係るSiC焼結体の接合体における接
合部を示す模式図である。
FIG. 2 is a schematic view showing a joint in a joined body of a SiC sintered body according to the present invention.

【符号の説明】[Explanation of symbols]

1 常圧焼結SiC焼結体 1a 開気孔 2 常圧焼結SiC焼結体 2a 開気孔 3 接合部 4 充填部 5 充填部 DESCRIPTION OF SYMBOLS 1 Normal pressure sintered SiC sintered compact 1a Open pore 2 Normal pressure sintered SiC sintered compact 2a Open pore 3 Joint 4 Filling part 5 Filling part

───────────────────────────────────────────────────── フロントページの続き (72)発明者 市島 雅彦 神奈川県秦野市曽屋30番地 東芝セラミッ クス株式会社開発研究所内 Fターム(参考) 4G026 BA14 BB14 BC01 BD14 BF01 BF42 BF44 BG02 BG23 BH06 5F004 AA14 AA15 BB29  ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Masahiko Ichijima 30 Soya, Hadano-shi, Kanagawa F-term in the development laboratory of Toshiba Ceramics Co., Ltd. 4G026 BA14 BB14 BC01 BD14 BF01 BF42 BF44 BG02 BG23 BH06 5F004 AA14 AA15 BB29

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 嵩密度2.8g/cm3 以上の常圧焼結Si
C焼結体同士がSiからなる接合部及び常圧焼結SiC
焼結体同士の接合面に開口する開気孔に充填されて接合
部と一体のSiからなる充填部を介して接合されている
ことを特徴とするSi焼結体の接合体。
Atmospheric pressure sintered Si having a bulk density of 2.8 g / cm 3 or more.
Joints of C sintered bodies made of Si and normal pressure sintered SiC
What is claimed is: 1. A bonded body of a Si sintered body, which is filled in open pores opened on a bonding surface between the sintered bodies and is bonded to the bonding part via a filling part made of Si.
【請求項2】 請求項1記載のSiC焼結体の接合体を
利用したことを特徴とする半導体製造用部材。
2. A member for manufacturing a semiconductor, wherein the bonded member of the SiC sintered body according to claim 1 is used.
【請求項3】 嵩密度2.8g/cm3 以上の常圧焼結Si
C焼結体の接合面にSiを載せ、非酸化性雰囲気又は真
空雰囲気においてSiの融点以上の温度で熱処理した
後、常圧焼結SiC焼結体同士の接合面間にSiを介在
し、非酸化性雰囲気又は真空雰囲気においてSiの融点
以上の温度で熱処理することを特徴とするSiC焼結体
の接合体の製造方法。
3. An atmospheric pressure sintered Si having a bulk density of 2.8 g / cm 3 or more.
After placing Si on the bonding surface of the C sintered body and performing a heat treatment at a temperature equal to or higher than the melting point of Si in a non-oxidizing atmosphere or a vacuum atmosphere, Si is interposed between the bonding surfaces of the normal pressure sintered SiC sintered bodies, A method for producing a joined body of SiC sintered bodies, wherein heat treatment is performed at a temperature equal to or higher than the melting point of Si in a non-oxidizing atmosphere or a vacuum atmosphere.
【請求項4】 前記Siが、板状、粒状又は粉状である
ことを特徴とする請求項3記載のSiC焼結体の接合体
の製造方法。
4. The method for producing a bonded SiC sintered body according to claim 3, wherein said Si is in the form of a plate, a particle, or a powder.
JP2000341881A 2000-11-09 2000-11-09 Jointed body of silicon carbide sintered compact, member for producing semiconductor using the same and method of producing the same Pending JP2002145677A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006282419A (en) * 2005-03-31 2006-10-19 Toshiba Ceramics Co Ltd Ceramic joined body
WO2016194444A1 (en) * 2015-06-01 2016-12-08 株式会社日立製作所 Silicon carbide ceramic assembly

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006282419A (en) * 2005-03-31 2006-10-19 Toshiba Ceramics Co Ltd Ceramic joined body
WO2016194444A1 (en) * 2015-06-01 2016-12-08 株式会社日立製作所 Silicon carbide ceramic assembly

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