JP6361505B2 - 不純物拡散組成物および半導体素子の製造方法 - Google Patents
不純物拡散組成物および半導体素子の製造方法 Download PDFInfo
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- JP6361505B2 JP6361505B2 JP2014531030A JP2014531030A JP6361505B2 JP 6361505 B2 JP6361505 B2 JP 6361505B2 JP 2014531030 A JP2014531030 A JP 2014531030A JP 2014531030 A JP2014531030 A JP 2014531030A JP 6361505 B2 JP6361505 B2 JP 6361505B2
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Description
(A)一般式(1)で表されるポリシロキサンと、(B)不純物拡散成分とを含有することを特徴とする不純物拡散組成物、である。
半導体基板に上記不純物拡散組成物を印刷して不純物拡散層膜を形成する工程と、前記不純物拡散層膜から不純物を拡散させて不純物拡散層を形成する工程を含む半導体素子の製造方法、である。
本発明の不純物拡散組成物において、不純物拡散成分は、半導体基板中に不純物拡散層を形成するための成分である。n型の不純物拡散成分としては、15族の元素を含む化合物であることが好ましく、中でもリン化合物であることが好ましい。p型の不純物拡散成分としては、13属の元素を含む化合物であることが好ましく、中でもホウ素化合物であることが好ましい。
BC:ブチルカルビトール
TERP:テルピネオール
PEO:ポリエチレンオキサイド
PMMA:ポリメチルメタクリレート
PPO:ポリプロピレンオキサイド
PVP:ポリビニルピロリドン
PVB:ポリビニルブチラール
EtOH:エタノール
PhTMS:フェニルトリメトキシシラン
PhTES:フェニルトリエトキシシラン
TolTMS:p−トリルトリメトキシシラン
MeOPhTMS:p−メトキシフェニルトリメトキシシラン
MeTMS:メチルトリメトキシシラン
EtTMS:エチルトリメトキシシラン
PrTMS:プロピルトリメトキシシラン
BuTMS:ブチルトリメトキシシラン
HexTMS:ヘキシルトリメトキシシラン
MePhDMS:メチルフェニルジメトキシシラン
PhEtTMS:2−フェニルエチルトリメトキシシラン
TEOS:テトラエトキシシラン。
粘度1,000mPa・s未満の不純物拡散組成物は、東機産業(株)製回転粘度計TVE−25L(E型デジタル粘度計)を用い、液温25℃、回転数20rpmでの粘度を測定した。また、粘度1,000mPa・s以上の不純物拡散組成物は、ブルックフィールド製RVDV−11+P(B型デジタル粘度計)を用い、液温25℃、各回転数での粘度を測定した。回転数20rpmでの測定値を粘度とし、回転数20rpmでの測定値(η20)と回転数2rpmでの測定値(η2)の比(η2/η20)をチクソ性とした。
(2−1)スリット塗布性
スリットノズルにより不純物拡散組成物をストライプ状にパターニングし、そのストライプ幅精度を確認した。
スクリーン印刷により不純物拡散組成物をストライプ状にパターニングし、そのストライプ幅精度を確認した。
3cm×3cmにカットしたn型シリコンウェハー((株)フェローテックシリコン製、表面抵抗率410Ω/□)を1%フッ酸水溶液に1分浸漬したあと水洗し、エアブロー後ホットプレートで140℃5分処理した。
n型不純物拡散組成物のp型不純物拡散組成物に対するマスク性を例にとって、マスク性測定方法について説明する。n型不純物拡散組成物からなる上記耐クラック膜厚観察基板(3cm×3cm)上にp型不純物拡散組成物PBF(東京応化工業(株)製)を半分程度(1.5cm×3cm)塗布し、200℃で10分間ホットプレートでプリベークした。その後、シリコンウェハーを電気炉内に配置し、窒素雰囲気下、900℃で60分間維持して不純物を熱拡散させた。熱拡散後、シリコンウェハーを、10重量%のフッ酸水溶液に23℃で1分間浸漬させて、硬化した拡散剤を剥離した。剥離後のシリコンウェハーに対して、表面抵抗を四探針式表面抵抗測定装置RT−70V(ナプソン(株)製)を用いて測定した。ここで、n型不純物拡散性組成物のみを塗布した領域の表面抵抗とn型不純物拡散性組成物上にp型不純物拡散組成物を塗布した領域の表面抵抗の差が±20%以内の場合、マスク性ありと判断した。マスク性がある最低マスク層膜厚サンプルの焼成後膜厚をマスク膜厚とした。
熱拡散後の各シリコンウェハーを、10重量%のフッ酸水溶液に23℃で1分間浸浸させて、拡散剤およびマスクを剥離した。剥離後、シリコンウェハーを純水に浸漬させて洗浄し、表面の目視により残渣の有無を観察した。1分浸漬後目視で表面付着物が確認でき、ウエスでこすっても除去できないものをworse(劣)、1分浸漬後目視で表面付着物が確認できるがウエスでこすることで除去できるものをbad(不可)、30秒を上回り1分以内で表面付着物が目視確認できなくなったものをgood(良)、30秒以内で表面付着物が目視確認できなくなったものをexcellent(優)とした。
3cm×3cmにカットしたn型シリコンウェハー((株)フェローテックシリコン製、表面抵抗率410Ω/□)を1%フッ酸水溶液に1分浸漬したあと水洗し、エアブロー後ホットプレートで140℃5分処理した。
不純物拡散組成物を冷蔵庫(4℃)で4週間保管し、4週間後の粘度が初期の粘度に対して、粘度変化3%未満の場合excellent(優)、3%以上6%未満の場合good(良)、6%以上10%未満の場合bad(不可)、粘度変化が10%以上もしくは沈殿、白濁、ゲル化などが起こった場合は、worse(劣)とした。
ポリシロキサン溶液の合成
500mLの三口フラスコにKBM−13(メチルトリメトキシシラン)を164.93g(1.21mol)、KBM−103(フェニルトリメトキシシラン)を204.07g(1.21mol)、GBLを363.03g仕込み、40℃で攪拌しながら水130.76gにリン酸0.1.215gを溶かしたリン酸水溶液を30分かけて添加した。滴下終了後、40℃で1時間撹拌した後、70℃に昇温し、30分撹拌した。その後、オイルバスを115℃まで昇温した。昇温開始1時間後に溶液の内温が100℃に到達し、そこから1時間加熱攪拌した(内温は100〜110℃)。得られた溶液を氷浴にて冷却し、ポリシロキサン溶液を得た。ポリシロキサン溶液の固形分濃度は39.8重量%であった。
表1記載の組成で調合し、不純物拡散組成物を得た。耐クラック性、マスク性、剥離性、パターン精度、保存安定性、シート抵抗値を測定したところ、表3に示すとおり、いずれも良好であった。特に、ポリシロキサン中の炭素数6〜15のアリール基の比率を増加したものでは、より大きい膜厚であってもクラックが入りにくく、耐クラック性が良好であった。
これらの実施例および参考例では各種増粘剤を溶液全体に対して所定の重量%濃度になるように添加し、自転・公転ミキサーARE−310((株)シンキー製)を用いて溶解させた(撹拌:15分、脱泡:1分)。耐クラック性、不純物拡散性、マスク性、剥離性、パターン精度、保存安定性、シート抵抗値を測定したところ、表3および表4に示すとおり、いずれも良好であった。ポリシロキサンの構成ユニットがすべて3官能性のオルガノシランであるものが、不純物拡散性、剥離性に優れていた。ポリシロキサン中のアリール基比率が40モル%以上のものが、不純物拡散性、マスク性に優れており、80モル%以下のものが、剥離性が特に良好であった。
n型不純物拡散層およびp型不純物拡散層形成方法
図6(a)に示すように、p型シリコンウェハー51((株)フェローテックシリコン製、表面抵抗率410Ω/□)上の一部にスクリーン印刷法により実施例1記載のn型不純物拡散組成物52を塗布した。塗布後、p型シリコンウェハー51を140℃5分間プリベークした。
n型不純物拡散層およびp型不純物拡散層形成方法
図7(a)に示すように、p型シリコンウェハー61((株)フェローテックシリコン製、表面抵抗率410Ω/□)上の一部にスクリーン印刷法により実施例1記載のn型不純物拡散組成物62を塗布した。塗布後、P型シリコンウェハー61を100℃5分間プリベークした。
表1および表2記載の組成で調合し、不純物拡散組成物を得た。なお、エチルシリケート48とはコルコート(株)製でテトラエトキシシランの加水分解縮合物(平均10量体)である。表3および表4に示すとおり、不純物拡散組成物の焼成膜は、耐クラック膜厚が極めて小さく、マスクマージンが極めて小さかった。
表2記載の組成で調合し、不純物拡散組成物を得た。表4に示すとおり、不純物拡散組成物の焼成膜は、耐クラック膜厚が極めて小さく、マスクマージンが極めて小さかった。また、保存安定性が悪く、4週間の冷蔵庫(4℃)保管でゲル化した。
表2記載の組成で調合し、不純物拡散組成物を得た。表4に示すとおり、不純物拡散組成物の焼成膜は、耐クラック膜厚が小さく、p型不純物拡散剤に対するマスク膜厚が大きいため、十分なマスクマージンが得られなかった。また、シート抵抗値も高く、保存安定性も悪かった。
表2記載の組成で調合し、不純物拡散組成物を得た。表4に示すとおり、不純物拡散組成物の焼成膜は、耐クラック膜厚が小さく、p型不純物拡散剤に対するマスク膜厚が大きいため、十分なマスクマージンが得られなかった。また、シート抵抗値も少し高く、保存安定性も悪かった。
表2記載の組成で調合し、不純物拡散組成物を得た。表4に示すとおり、不純物拡散組成物の焼成膜は、剥離性が悪く残渣が残ったため、シート抵抗値が高かった。
表2記載の組成で調合し、不純物拡散組成物を得た。表4に示すとおり、不純物拡散組成物の焼成膜は、耐クラック膜厚が小さく、p型不純物拡散剤に対するマスク膜厚が少し大きいため、十分なマスクマージンが得られなかった。また、剥離性が悪く残渣が残ったため、シート抵抗値が高かった。
2 n型不純物拡散組成物
3 n型不純物拡散層
4 p型不純物拡散組成物
5 p型不純物拡散層
6 保護膜
6a 保護膜開口
7 n型コンタクト電極
8 p型コンタクト電極
9 裏面接合型太陽電池
30 ストライプ塗布装置
31 半導体基板
32 ステージ
33 リニア駆動装置(X方向)
34 リニア駆動装置(Y方向)
35 ブラケット
36 CCDカメラ
37 高さセンサー
38 ノズル
40 半導体基板
41 ノズル
42 吐出口
43 ペースト
44 ビード
45 マニホールド
46 加圧口
47 ペースト供給口
51 p型シリコンウェハー
52 n型不純物拡散組成物
53 n型不純物拡散層
54 p型不純物拡散組成物
55 p型不純物拡散層
61 p型シリコンウェハー
62 n型不純物拡散組成物
63 n型不純物拡散層
64 p型不純物拡散組成物
65 p型不純物拡散層
Claims (6)
- 前記(A)ポリシロキサンの20%熱分解温度が550℃以上である請求項1記載の不純物拡散組成物。
- さらに(C)増粘剤を前記組成物に対し3重量%以上20重量%以下含有する請求項1または2記載の不純物拡散組成物。
- 半導体基板に請求項1〜3のいずれかに記載の不純物拡散組成物を印刷して不純物拡散組成物膜を形成する工程と、前記不純物拡散組成物膜から不純物を拡散させて不純物拡散層を形成する工程を含む半導体素子の製造方法。
- 前記不純物拡散組成物膜が不純物拡散組成物パターンである請求項4記載の半導体素子の製造方法。
- 前記印刷がスクリーン印刷である請求項4または5記載の半導体素子の製造方法。
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