JP4921150B2 - 窒化アルミニウム接合体の製造方法 - Google Patents
窒化アルミニウム接合体の製造方法 Download PDFInfo
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Description
本発明の実施形態による接合材は、融材と窒化アルミニウム(AlN)粉末とを含んでおり、窒化アルミニウムを含む取付体及び被取付体同士の接合に好適に用いることができる。
融材は、酸化カルシウムアルミニウム(CaxAlyOz)、又は、酸化カルシウム(CaO)及び酸化アルミニウム(Al2O3)を含む。即ち、融材は、少なくとも酸化カルシウムアルミニウムを含んでいるか、あるいは、酸化カルシウムと酸化アルミニウムの両方を含んでいる。そのため、融材は、酸化カルシウムアルミニウムだけを含む、酸化カルシウムアルミニウムと酸化カルシウムを含む、酸化カルシウムアルミニウムと酸化アルミニウムを含む、酸化カルシウムアルミニウムと酸化カルシウムと酸化アルミニウムを含む、酸化カルシウムと酸化アルミニウムを含むことが好ましい。
本実施形態に係る窒化アルミニウム接合体1は、図1に示すように、細長い円柱状(棒状)に形成された窒化アルミニウムを主成分とする取付体3と、支持穴5に取付体3の先端部3aを螺合及び接合した窒化アルミニウムを主成分とする被取付体7と、被取付体7の支持穴5の底面9全体に配設された接合層11とを備える。この接合層11は、窒素(N)、酸素(O)、アルミニウム(Al)、カルシウム(Ca)を含み、希土類元素の含有量が15重量%未満である。なお、接合層11に含まれる希土類元素は、もともと接合材に含まれているか、また、接合される対象物である取付体3や被取付体7中の窒化アルミニウムに含まれている希土類元素が接合層11に入り込む。また、希土類元素が全く含まれていなくても良い。
本発明の実施形態による窒化アルミニウム接合体の製造方法について、図2を参照して説明する。
被取付体27の支持穴25の側面には、めねじが切ってある。まず、支持穴25の底面29から底面29近傍の側面にかけて接合材を塗布する。また、支持穴25の底面29の平均表面粗さは、0.4〜1.6μmである。
次いで、取付体23の先端部23aを被取付体27の支持穴25に螺合させる。この先端部23aの外周には、おねじが切ってあり、被取付体27の支持穴25のめねじに螺合可能に形成されている。取付体23を螺合させていき、先端部23aの先端面23bが支持穴25内の接合材に当接させる。このように、本実施形態においては、取付体23を被取付体27に対して加圧する必要がない。また、取付体23の先端部23aの平均表面粗さは、0.4〜1.6μmである。
この状態で、取付体23及び被取付体27を窒素ガスやアルゴンガス等の不活性ガス雰囲気中又は減圧雰囲気中に配置し、1500℃以下の接合温度で加熱する。これによれば、低い接合温度で良好な接合状態を得ることができ、窒化アルミニウムを含む取付体及び被取付体の熱変形を小さくすることができる。接合温度は、1400〜1500℃であることがより好ましい。取付体23や被取付体27の大きさや形状にもよるが、1500℃以下で5分〜3時間保持することが好ましい。
実施例1を説明する。まず、本発明例1による窒化アルミニウム接合体について詳述する。
最初に、窒化アルミニウム粉末95重量%に、焼結助剤として酸化イットリウム5重量%を加え、ボールミルを用いて混合した。得られた混合粉末に、バインダを添加し、噴霧造粒法により造粒した。得られた造粒粉を金型成形及びCIPにより板状成形体と管状成形体とを成形した。得られた板状成形体(被取付体)を窒素ガス中でホットプレス法により、管状成形体(取付体)を窒素ガス中で常圧焼成により1860℃で6時間焼成した。このホットプレス焼成によって、前記板状成形体は板状焼成体となり、管状成形体は管状焼成体となった。
酸化カルシウム(CaO)50重量%と酸化アルミニウム(Al2O3)50重量%からなる融材と、イットリウム(Y)を5重量%含む窒化アルミニウム粉末とを、PVAおよびエタノールに混合させてペーストにした接合材を作成した。前記板状焼成体の支持穴の底面に、接合材の量が14mg/cm2となるように接合材を均一に塗布した。
前述した本発明例1による窒化アルミニウム接合体の接合部分について、強度及び気密性を評価した。強度は、JIS R1601に従い、室温で4点曲げ強度を測定した。強度は、耐久性試験前(以下「初期状態」という)、耐久性試験後にそれぞれ測定した。耐久性試験は、大気中において、窒化アルミニウム接合体を昇温速度を10℃/分として800℃まで加熱し、室温まで冷却する処理を100回繰り返して行った。
また、比較例1においては、前記本発明例1と同様にして、板状焼成体と管状焼成体を作成し、管状焼成体を接合層を介して板状焼成体に接合させた。ただし、管状焼成体の先端部には、おねじを形成せず、板状焼成体の支持穴にもめねじを形成しなかった。
次に、実施例2を説明する。この実施例2は、実施例1に対して、接合材中における融材の組成のみを変えており、他の条件(例えば、窒化アルミニウム接合体の製造方法等)は全て実施例1と同一とした。
次に、実施例3について説明する。この実施例3は、実施例1に対して、図2に示す先端面23b及び底面29の表面粗さのみを変えており、他の条件(例えば、窒化アルミニウム接合体の製造方法等)は全て実施例1と同一とした。
3,23,52,82…取付体
3a,23a…先端部
5,25,56…支持穴
7,27,53,62,83,…被取付体
11…接合層
31,86…貫通孔
33…挿通孔
41…加熱装置
42…円盤状部材(被取付体)
43…管状部材(取付体)
Claims (3)
- 窒化アルミニウムを含む棒状の取付体、及び窒化アルミニウムを含む被取付体の少なくともいずれかに接合材を塗布するステップと、
前記取付体を被取付体の支持穴に螺合させて、前記取付体を前記接合材を介して被取付体に圧接させるステップと、
前記取付体、接合材及び被取付体を1500℃以下の接合温度で加熱することにより、取付体を接合層を介して被取付体に接合させるステップとを有し、
前記接合材は、酸化カルシウムアルミニウム、又は、酸化カルシウム及び酸化アルミニウムを含み、希土類元素が5重量%未満である融材と、窒化アルミニウム粉末とを含むことにより、
取付体と被取付体との当接部のうち、少なくとも、前記螺合によって取付体が被取付体から圧接力を受ける圧接部を接合層を介して互いに接合させる窒化アルミニウム接合体の製造方法。 - 前記取付体と被取付体との当接部のうち、少なくとも、前記螺合によって圧接力を受ける圧接部の平均表面粗さが0.4〜1.6μmであることを特徴とする請求項1に記載の窒化アルミニウム接合体の製造方法。
- 昇温速度を0.5〜10.0℃/分として前記接合温度まで昇温することを特徴とする請求項1又は2に記載の窒化アルミニウム接合体の製造方法。
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US9624137B2 (en) * | 2011-11-30 | 2017-04-18 | Component Re-Engineering Company, Inc. | Low temperature method for hermetically joining non-diffusing ceramic materials |
US9315424B2 (en) * | 2011-11-30 | 2016-04-19 | Component Re-Engineering Company, Inc. | Multi-layer plate device |
US8932690B2 (en) * | 2011-11-30 | 2015-01-13 | Component Re-Engineering Company, Inc. | Plate and shaft device |
WO2016005557A1 (de) * | 2014-07-10 | 2016-01-14 | Ceramtec Gmbh | Keramischer laminierter formkörper mit aussparungen |
JP2023056156A (ja) * | 2021-10-07 | 2023-04-19 | 日本碍子株式会社 | 半導体製造装置用部材 |
CN114749754B (zh) * | 2022-05-31 | 2023-07-25 | 核工业西南物理研究院 | 一种用于真空钎焊工艺评定的真空钎焊评定试件 |
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JP2783980B2 (ja) * | 1994-09-01 | 1998-08-06 | 日本碍子株式会社 | 接合体およびその製造方法 |
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EP1803696A1 (en) | 2007-07-04 |
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