JPWO2010002001A1 - 窒化珪素基板及びその製造方法並びにそれを使用した窒化珪素回路基板及び半導体モジュール - Google Patents
窒化珪素基板及びその製造方法並びにそれを使用した窒化珪素回路基板及び半導体モジュール Download PDFInfo
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Abstract
Description
また、透過型電子顕微鏡(Transmission Electron Microscope:TEM)を用いた観察により粒界相中における結晶相の析出有無を確認し、粒界相(非晶質相と粒界結晶相の和)中における結晶相の存在比率(面積率)について画像解析により算出した。
また、焼結助剤として添加するMgO粉末およびY2O3粉末は、それぞれ、平均粒子径を1.0μm以下、比表面積を30m2/g以下の範囲とする。また、不純物量は窒化珪素粉末と同様にFe成分およびAl成分は、それぞれ1000ppm以下とする。
まず、原料調整・混合工程として、含有酸素量2質量%以下の窒化珪素原料粉に酸化マグネシウム(MgO)が6.7〜12.8mol%、少なくとも1種の希土類元素酸化物(RE2O3)が1.1〜2.9mol%を合計7.9〜15.1mol%、かつ(RE2O3)/(MgO)のモル比が0.09〜0.3となるように混合し、溶剤、有機バインダー、可塑剤等とともにボールミル等で混合する。MgO、RE2O3及び合計の添加量と(RE2O3)/(MgO)の添加量のモル比が上記範囲以外の場合、MgO、RE2O3及び合計の含有量と(RE2O3)/(MgO)の含有量のモル比も上記範囲外となり、上述したように曲げ強度と熱伝導率の一方もしくは両方が低下する。従って、MgO、RE2O3、その合計の添加量及び(RE2O3)/(MgO)のモル比は上記範囲が好適である。
Ion Beam:FIB、日立製作所製 FB-2100)を用いて薄片化試料を作製し、続いて、透過型電子顕微鏡(TEM、日立製作所製 HF2000)を用いて行った。TEM観察条件は加速電圧200kV、直接観察倍率20k倍である。図2のTEM像を画像解析装置(ニレコ社製 ルーゼックスAP)を用いて粒界結晶相の存在比率(面積率)を算定したところ、その値は9.33%であった。粒界結晶相の存在比率は粒界結晶相の面積を粒界相(粒界結晶相と非晶質相の和)の面積で除して100を乗じて得られる値である。これと同様に実施例1〜3および実施例5〜9さらに表2−1および表2−2のおいて、X線回折により粒界結晶相の回折ピークが検出できた比較例1、2、7、8、10、11および14について同様の評価を行い、いずれの場合も粒界結晶相の存在比率を求めた。なお、比較例1,2,7,8,10および11の試料については、X線回折によりMgSiN2相に加えてY2Si3O3N4の回折ピークが検出されたが、TEM観察とTEM−EDX分析の結果からもMgが主成分である粒界結晶相とYが主成分のものの析出が確認できた。比較例1、2、7、8、10および11についてのMgSiN2相の存在比率は、MgSiN2相の面積を粒界相(これらの場合は、MgSiN2とY2Si3O3N4と非晶質相の和)で除して100を乗じて算出した。表5および図6に、MgSiN2結晶相の(121)のX線回折ピーク強度のβ型Si3N4前記β型窒化珪素の結晶粒子の(110)、(200)、(101)、(210)、(201)、(310)、(320)及び(002)のX線回折ピーク強度の和に対する比率(表3中では、単にMgSiN2X線比率と表記)とTEM像の画像解析により求めた粒界結晶相MgSiN2の存在比率の関係を示す。これらの図表から、実施例1〜9の場合、MgSiN2のX線比率は、0.0005〜0.003の範囲にあり、粒界相におけるMgSiN2の存在比率は、0.05%以上、20%未満の範囲にあった。また、図6よりMgSiN2のX線比率と粒界相におけるMgSiN2の存在比率との間には相関性があり、実施例1の0.0005で0.05%、実施例4の0.0017で7.62%、実施例6の0.003で18.54%および比較例0.0045で32.12%となった。
MgOおよびY2O3ともに添加量増大により粒界相中に過剰のMgSiN2結晶相が析出しやすくなり、MgSiN2結晶相の(121)のX線回折ピーク強度のβ型Si3N4前記β型窒化珪素の結晶粒子の(110)、(200)、(101)、(210)、(201)、(310)、(320)及び(002)のX線回折ピーク強度の和に対する比率は0.0035と増大し、βSi3N4粒子との結合強度の小さい粒界結晶相の存在比率が増加したため窒化珪素基板の曲げ強度は低下した。
11 窒化珪素粒子
12 非晶質の粒界相
13 結晶質の粒界相
Claims (6)
- β型窒化珪素の結晶粒子と、少なくとも1種類の希土類元素(RE)、マグネシウム(Mg)及び珪素(Si)を含有する粒界相からなる窒化珪素基板において、前記粒界相は非晶質相とMgSiN2結晶相からなり、前記希土類元素(RE)を含んだ結晶相のいずれの結晶面のX線回折線ピーク強度も前記β型窒化珪素の結晶粒子の(110)、(200)、(101)、(210)、(201)、(310)、(320)及び(002)の回折線ピーク強度の和の0.0005倍未満であり、前記MgSiN2結晶相の(121)のX線回折ピーク強度が前記β型窒化珪素の結晶粒子の(110)、(200)、(101)、(210)、(201)、(310)、(320)及び(002)のX線回折ピーク強度の和の0.0005〜0.003倍であることを特徴とする窒化珪素質焼結体。
- 熱伝導率が80W/m・K以上である請求項1記載の窒化珪素質焼結体。
- 前記窒化珪素基板が含有するマグネシウム(Mg)を酸化マグネシウム(MgO)に換算し、同じく含有する少なくとも1種類の希土類元素(RE)を希土類元素酸化物(RE2O3)に換算したとき、MgO含有量が6.7〜12.8mol%、RE2O3含有量が1.1〜2.9mol%、MgOとRE2O3の含有量の合計が7.9〜15.1mol%で、かつ(RE2O3)/(MgO)のモル比が0.09〜0.3であることを特徴とする請求項1または2に記載の窒化珪素質焼結体。
- 含有酸素量2.0質量%以下の窒化珪素原料粉に、酸化マグネシウム(MgO)を6.7〜12.8mol%と少なくとも1種類の希土類元素酸化物(RE2O3)を1.1〜2.9mol%とを合計7.9〜15.1mol%、かつ(RE2O3)/(MgO)のモル比が0.09〜0.3になるように配合して総厚み40mm以下のシート成形体とし、前記シート成形体を1600℃から300℃/h以下の速度で1800〜2000℃の温度に昇温し、2〜10時間保持した後、100℃/h以上の速度で1500℃まで冷却することで焼結することを特徴とする窒化珪素質焼結体の製造方法。
- 請求項1乃至3の何れかに記載の窒化珪素質焼結体からなる窒化珪素基板と、前記窒化珪素基板の一面に接合された金属回路板と、前記窒化珪素基板の他の面に接合された金属放熱板とからなることを特徴とする窒化珪素回路基板。
- 請求項5に記載の窒化珪素回路基板と、該窒化珪素回路基板上に搭載された半導体素子を有することを特徴とする半導体モジュール。
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