JP7313105B2 - 構造体及び接合体 - Google Patents
構造体及び接合体 Download PDFInfo
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Description
図1は、実施形態に係る構造体を例示する模式的断面図である。
実施形態に係る構造体110は、図1に示すように、結晶粒10と、結晶粒10の周りに設けられた粒界20と、を含む。結晶粒10は、粒界20中に複数存在する。粒界20中の複数の結晶粒10は、互いに離れて存在しても良いし、互いに部分的に接していても良い。複数の結晶粒10の一部が互いに離れ、複数の結晶粒10の別の一部が互いに部分的に接していても良い。
図2は、実施形態に係る構造体のθ-2θ法によるX線回折パターンを示す。横軸は、2θを表す。縦軸は、正規化された強度を表す。
X線回折パターンの測定時の条件は、例えば以下のように設定される。X線回折装置、例えば(株)リガク製Smart-Labを用い、集中法(反射法、Bragg-Brendano法)によるX線回折を行う。X線回折では、構造体の任意の断面を測定面とする。測定面は、表面粗さRaが0.05μm以下となるように研磨する。測定には、Cuターゲット(Cu-Kα)を使用する。管電圧は、45kVに設定する。管電流は、200mAに設定する。走査速度は、2.0~20.0°/minに設定する。入射平行スリットを5度、長手制限スリットを10mm、受光スリットを20mm、受光平行スリットを5度に設定する。走査範囲(2θ)は、10°~80°に設定し、0.01°刻みで測定する。
SiをSi3N4換算で100mol%、Y2O3を2mol%、MgOを5mol%秤量する。Y2O3及びMgOは、助剤として用いられる。助剤としては他にもB2O3を用いることができ、これらは単独で用いてもよいし、複数を混合して用いてもよい。助剤の割合はSi3N4換算で2mol%以上20mol%以下であることが好ましい。
これらの材料を遊星ボールミルにて0.2時間以上6時間以下解砕して混合する。粉砕時間が短すぎると材料の粒径が大きすぎ、構造体の強度が低下するため好ましくない。粉砕時間が長すぎると材料の粒径が小さくなりすぎ、熱伝導率が低下するため好ましくない。
次に、混合物を乾燥させ、バインダを加えて造粒する。このとき、バインダとしてはポリビニルブチルアルコールやアクリル樹脂などを用いることができる。これらのバインダは、単独で用いてもよいし、複数を混合して用いてもよい。バインダは総量に対して1wt%以上20wt%以下加えることが好ましい。バインダが1wt%より少ないと材料どうしが結着しにくくなり強度が構造体の低下するため好ましくない。バインダが20wt%より多いと構造体中のバインダの量が多くなりすぎ、構造体の熱伝導率が低下するため好ましくない。
その後、0.5t/cm2以上10t/cm2以下の圧力を加えて成型する。圧力は材料に合わせて調整する。成型体を300℃以上800℃以下にて空気中で脱脂した後、窒素雰囲気において1000℃以上1500℃以下で処理する。脱脂及び窒素雰囲気における処理時間は、処理温度に応じて調整する。
その後、1700℃以上2100℃以下で1時間以上200時間以下焼結を行うことで、実施形態に係る構造体が得られる。
SiをSi3N4換算で100mol%、Y2O3を2mol%、MgOを5mol%秤量する。Y2O3及びMgOは、助剤として用いられる。これらの材料を遊星ボールミルにて1時間解砕して混合する。混合物を乾燥させ、5wt%のポリビニルブチルアルコールをバインダとして加えて造粒する。その後、1t/cm2の圧力を加えて成型する。成型体を500℃にて空気中で脱脂した後、窒素雰囲気において1400℃で8時間処理する。その後、1900℃で24時間焼結を行い、焼結体を作製する。これにより、実施形態に係る構造体が得られる。
試料2の製造では、試料1の製造と原料混合時間が異なる。試料3の製造では、試料1の製造と助剤の割合が異なる。これらの点を除いて、試料2及び3は、試料1と同様に作製した。
図3~図5は、参考例に係る構造体のθ-2θ法によるX線回折パターンを示す。横軸は、2θを表す。縦軸は、正規化された強度を表す。図3~図5の上段のグラフは、試料の分析結果を示す。図3~図5の下側(紙面右側)のグラフは、試料の分析結果を示す。
曲げ強度は、JIS-R-1601に準じて3点曲げ強度試験により測定される。JIS-R-1601は、ISO14704(2000)に対応する。3点曲げ強度試験には、島津製作所製 オートグラフ AG-X(100kN)を用いる。ロードセルを1kN、試験速度を0.5mm/min、圧子半径および支持台半径を共にR2、支点間距離を30mmに設定し、室温で実施する。
また、実施形態に係る構造体の曲げ強度は、第2参考例又は第3参考例に係る構造体の熱伝導率よりも高い。第1参考例に係る構造体の曲げ強度は、実施形態に係る構造体の曲げ強度よりも高い。しかし、第1参考例に係る構造体の熱伝導率は、実施形態に係る構造体の熱伝導率よりも劣る。
すなわち、実施形態に係る構造体は、熱伝導率及び曲げ強度の両方において優れる。例えば、実施形態によれば、構造体の熱伝導率を100(m・K)以上、且つ曲げ強度を300MPa以上にできる。
例えば図6(a)及び図6(b)に示すように、実施形態に係る構造体は、基板である。基板の形状は、任意である。上述した通り、実施形態に係る構造体は、高い熱伝導率及び高い曲げ強度を有する。このため、実施形態に係る構造体は、基板に好適に用いることができる。又は、実施形態に係る構造体は、ベアリング等であっても良い。
実施形態に係る接合体210は、図7に示すように、第1金属部31及び構造体110を含む。この例では、構造体110は、基板として用いられる。
Claims (11)
- β型窒化珪素型結晶相およびY2Si3O3N4型結晶相を含み、
θ-2θ法によるX線回折パターンにおいて、2θ=27.03±0.1°に現れる最大の第1ピーク強度に対する、2θ=31.93±0.1°に現れる最大の第2ピーク強度の比が、0.005以上0.20以下である構造体。 - 前記X線回折パターンにおいて、2θ=33.63±0.1°に現れる最大の第3ピーク強度に対する、2θ=29.67±0.1°に現れる最大の第4ピーク強度の比が、0.00以上0.20以下である請求項1記載の構造体。
- 前記第1ピーク強度に対する前記第2ピーク強度の比は、0.005以上0.17以下である請求項1又は2に記載の構造体。
- 前記X線回折パターンにおいて、2θ=36.04±0.1°に現れる最大の第5ピーク強度に対する、2θ=38.36±0.1°に現れる最大の第6ピーク強度の比が、0.00以上0.20以下である請求項1~3のいずれか1つに記載の構造体。
- 2θ=31.93±0.1°に現れる前記第2ピークの半値全幅は、0.25°以下である請求項1~4のいずれか1つに記載の構造体。
- 前記β型窒化珪素型結晶相を含む結晶粒と、
前記結晶粒の周りに設けられ、前記Y2Si3O3N4型結晶相を含む粒界と、
を含む請求項1~5のいずれか1つに記載の構造体。 - 熱伝導率が100W/(m・K)以上であり、
曲げ強度が300MPa以上である請求項1~6のいずれか1つに記載の構造体。 - 請求項1~7のいずれか1つに記載の構造体を用いた基板と、
前記基板に接合された第1金属部材と、
を備えた接合体。 - 前記基板と前記第1金属部材は、第1接合部を介して接合され、
前記第1金属部材は、銅を含み、
前記第1接合部は、銀と、銅と、チタン、ハフニウム、ジルコニウム、ニオブ、シリコン、マグネシウム、インジウム、錫、及び炭素からなる群より選択される少なくとも1つと、を含む請求項8記載の接合体。 - 前記基板に接合された第2金属部材をさらに備え、
前記基板は、前記第1金属部材と前記第2金属部材との間に位置する請求項8又は9に記載の接合体。 - 前記第1金属部材と接合された半導体素子をさらに備え、
前記第1金属部材は、前記基板と前記半導体素子との間に位置する請求項8~10のいずれか1つに記載の接合体。
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