JPWO2007004579A1 - セラミックシートの製造方法、それを用いたセラミック基板及びその用途 - Google Patents
セラミックシートの製造方法、それを用いたセラミック基板及びその用途 Download PDFInfo
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Abstract
Description
本発明の目的は、ボイドを低減することにより品質の安定した高信頼性セラミックシートの製造方法、及びそれを用いたセラミック基板を提供することである。
(1)セラミック粉末、焼結助剤、及びヒドロキシプロピルメチルセルロースを含む混合粉末に、水、離型剤及び可塑剤を含む混合液を噴霧して粒状の湿紛原料を作製し、該湿紛原料を混練し、次いで、シートダイスを取付けた一軸成形機によりシート成形を行うことを特徴とするセラミックシートの製造方法。
(2)前記混合粉末においてセラミック粉末100質量部に対し、ヒドロキシプロピルメチルセルロースが5〜15質量部及び焼結助剤が1〜15質量部含まれる上記(1)に記載のセラミックシートの製造方法。
(3)前記湿紛原料を、二軸押出機にて混練する上記(1)又は(2)に記載のセラミックシートの製造方法。
(4)前記セラミック粉末が、窒化硅素粉末である上記(1)〜(3)のいずれかに記載のセラミックシートの製造方法。
(5)ヒドロキシプロピルメチルセルロースが、メトキシ基を19〜30質量%及びヒドロキシプロポキシル基を4〜12質量%含有する上記(1)〜(4)のいずれかに記載のセラミックシートの製造方法。
(6)上記(1)〜(5)のいずれかに記載の製造方法により得られたセラミックシートに、脱脂及び焼結処理を施してなるセラミック基板。
(7)ボイド率が3体積%以下である上記(6)に記載のセラミック基板。
(8)上記(6)又は(7)に記載のセラミック基板の一主面に金属回路を形成し、他の一主面に放熱板を接合してなるセラミック回路基板。
(9)10pC以上の部分放電開始電圧が5KV以上である上記(8)に記載のセラミック回路基板。
(10)上記(8)又は(9)に記載のセラミック回路基板を用いてなるモジュール。
1 定量フィーダー
2 二軸押出機変速モーター
3 湿粉投入口
4 二軸押出機本体
5 乾式真空ポンプ
6 二軸押出機用真空計
7 練土排出口
8 真空室
9 一軸成形機側真空コック
10 一軸成形機用真空計
11 押出荷重圧計
12 シートダイス
13 シート押出口(口金)
14 一軸成形機本体
15 一軸成形機変速モーター
16 冷却用チラーユニット
1 定量フィーダー
2 二軸押出機変速モーター
3 湿粉投入口
4 二軸押出機本体
5 冷却用チラーユニット
6 乾式真空ポンプ
7 練土排出口
8 真空計
1 練土投入口
2 一軸成形機本体
3 予備混練真空室
4 乾式真空ポンプ
5 真空計
6 押出荷重圧計
7 シート押出口(口金部)
8 シートダイス
9 冷却用チラーユニット
焼結助剤の使用量は、セラミック粉末100質量部に対して好ましくは1〜15質量部、特に好ましくは4〜10質量部が好適である。使用量が1質量部未満であったり、或いは、15質量部を超えると、高密度な焼結体が得られない場合がある。本発明では、前記焼結助剤の他に、さらにアルカリ土類金属類の酸化物及び/又は珪素酸化物を併用し、焼成温度を低下させることはより好ましい。アルカリ土類金属類の酸化物及び/又は珪素酸化物の使用量は、セラミック粉末100質量部に対して0.1〜5質量部が好ましい。
本発明では、セラミック粉末、焼結助剤及びヒドロキシプロピルメチルセルロースを含む混合粉末には、精製グリセリン、グリセリントリオレート、ジエチレングリコール等の可塑剤や、ステアリン酸系やシリコン系等の離型剤、さらに必要に応じて分散剤を適宜配合することが好ましい。それらの含有量は、各々、セラミック粉末100質量部に対し外割配合で0.1〜5質量部が好ましい。
なお、上記の混合液に含有される、離型剤としては、脂肪酸エステル型、エマルジョン型、カルシウム型などのステアリン酸系化合物や、脂肪酸を含むシリコン系化合物等が使用される。また、可塑剤としては、精製グリセリン、グリセリントリオレート、ジエチレングリコール等が使用される。また、水は、純水またはイオン交換水が好ましく使用される。混合液中の離型剤及び可塑剤の含有量は、いずれも、セラミック粉末100質量部に対して、好ましくは2〜12質量%、特に好ましくは3〜6質量%である。
セラミック基板と金属板又は金属回路との接合は、例えば、Al−Cu、Ag、Cu、又はAg−Cu合金と、例えば、Ti、Zr、Hf等の活性金属成分を含むロウ材を介在させ、不活性ガス又は真空雰囲気中で加熱する方法や、Al−Mg等のAl合金箔を介在させ、真空中で加熱する方法により可能である。次いで回路面に、フォトレジストやスクリーン印刷等によりエッチングレジストを回路形状に印刷し、塩化銅、塩化鉄、アンモニア水、硫酸−過酸化水素等をエッチャントとしたエッチング処理を行うことで、セラミック回路基板を作製することができる。
〈実験No.1〜13〉
下記のSN粉末100質量部に対して、オレイン酸を3質量部添加し、ミキサー混合により表面処理をおこなったSN粉末100質量部に対し、Y2O35.5質量部、MgO.3質量部及びヒドロキシプロピルメチルセルロースをボールトン混合機により混合した。次いで、得られた混合物をミキサーに投入し、撹拌しながら、該混合物に対して、下記の可塑剤、離型剤及びイオン交換水からなる混合溶液を、SN粉末100質量部に対して可塑剤が3質量部(外割)、離型剤が3質量部(外割)、イオン交換水が18質量部となるように圧縮空気(0.2MPa)にて噴霧することにより、顆粒状の湿粉原料を調製した。
〈使用原料〉
・SN粉末:α化率90%、D50値0.7μm、D90値2.0μm、D100値4.6μm、比表面積12m2/g。
・Y2O3:信越化学工業株式会社製、商品名「Yttrium Oxide」、D50粉末粒径1.0μm。
・MgO:岩谷化学株式会社製、商品名「MTK−30」、D50粉末粒径0.2μm、比表面積160m2/g。
・ヒドロキシプロピルメチルセルロース:信越化学工業株式会社製、商品名「メトローズ・60SH、65SH、90SH」。
・可塑剤:花王社製、商品名「エキセパール」、主成分グリセリン。
・離型剤:サンノプコ社製、商品名「ノプコセラLU−6418」、主成分ステアリン酸。
この接合体の一方の主面には所定の形状の回路パターンを、他方の主面には放熱板パターンを形成させるべく、UV硬化型レジストインクをスクリーン印刷した後、UVランプを照射させてレジスト膜を硬化させた。次いで、レジスト塗布した部分以外を塩化第二銅溶液でエッチングした後、フッ化アンモニウム水溶液にてレジスト剥離し、銅回路SN基板を作製し、部分放電開始電圧の測定をおこなった。結果を表1に示す。
・銅板:、無酸素銅板(住友金属鉱山伸銅株式会社製、JIS H 3100)
・UV硬化型レジストインク:互応化学工業株式会社製「PER−27B−6」
〈測定方法〉
・Ti値:試料ホルダーを10℃に保持された降下式フローテスター「(株)島津製作所社製 CFT−100D」にて、せん断応力0.3MPa時の粘度と0.9MPa時の粘度の比を求めた。
・押出荷重圧:シートダイスに取り付けた口金を調整し、0.5mm×80mmの長方形の形状の開口部よりシート成形時の押出荷重圧を測定した。
・シート寸法:マイクロメーターを用いて、シート幅方向の厚みを測定した(n=5平均値)。
・シート強度:幅10mm、長さ40mmのシート強度を、JIS K6251「引っ張り試験方法」に準拠して測定した。
・クラック発生角度:シートを最大120°まで折り曲げ、シートにクラックのはいる角度を測定した。
・焼結体の抗折強度:下部スパン30mm、クロスヘッド速度0.5mm/分の条件にて3点曲げ試験(JIS R1601)より求めた(n=5平均値)。
・ボイド率:セラミックス焼結体を厚みの半分まで研磨し、電子顕微鏡にて直径15μm以上のボイドについて、その直径を測定し、下式により計算によって求めた。(n=3平均値)
ボイド率(体積%)=Σ(4/3πr3)/(W×L×t)×100
ここで、r:ボイド径(mm)、W:焼結体の幅(mm)、L :焼結体の長さ(mm)、t:焼結体の厚み(mm)である。
・部分放電開始電圧:作製した回路基板を絶縁油(住友3M社製「フロリナートFC−77」)に浸漬して、1kV/分のスピードで電圧を印可したとき、部分放電電荷量が10pCを超した時の電圧を、部分放電開始電圧とした(n=5平均値)。
〈実験No.14、15〉
二軸押出機の代わりに、三本ロール混練機、単軸押出機のみを用いたこと以外は、実施例1と同様に行った。結果を表1に示す。
なお、2005年7月4日に出願された日本特許出願2005−194750号の明細書、特許請求の範囲、図面及び要約書の全内容をここに引用し、本発明の明細書の開示として、取り入れるものである。
Claims (10)
- セラミック粉末、焼結助剤、及びヒドロキシプロピルメチルセルロースを含む混合粉末に、水、離型剤及び可塑剤を含む混合液を噴霧して粒状の湿紛原料を作製し、該湿紛原料を混練し、次いで、シートダイスを取付けた一軸成形機によりシート成形を行うことを特徴とするセラミックシートの製造方法。
- 前記混合粉末においてセラミック粉末100質量部に対し、ヒドロキシプロピルメチルセルロースが5〜15質量部及び焼結助剤が1〜15質量部含まれる請求項1に記載のセラミックシートの製造方法。
- 前記湿紛原料を、二軸押出機にて混練する請求項1又は2に記載のセラミックシートの製造方法。
- 前記セラミック粉末が、窒化硅素粉末である請求項1〜3のいずれかに記載のセラミックシートの製造方法。
- ヒドロキシプロピルメチルセルロースが、メトキシ基を19〜30質量%及びヒドロキシプロポキシル基を4〜12質量%含有する請求項1〜4のいずれかに記載のセラミックシートの製造方法。
- 請求項1〜5のいずれかに記載の製造方法により得られたセラミックシートに、脱脂及び焼結処理を施してなるセラミック基板。
- ボイド率が3体積%以下である請求項6に記載のセラミック基板。
- 請求項6又は7に記載のセラミック基板の一主面に金属回路を形成し、他の一主面に放熱板を接合してなるセラミック回路基板。
- 10pC以上の部分放電開始電圧が5KV以上である請求項8に記載のセラミック回路基板。
- 請求項8又は9に記載のセラミック回路基板を用いてなるモジュール。
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