JP6855794B2 - 不純物拡散組成物、それを用いた半導体素子の製造方法および太陽電池 - Google Patents
不純物拡散組成物、それを用いた半導体素子の製造方法および太陽電池 Download PDFInfo
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- JP6855794B2 JP6855794B2 JP2016504239A JP2016504239A JP6855794B2 JP 6855794 B2 JP6855794 B2 JP 6855794B2 JP 2016504239 A JP2016504239 A JP 2016504239A JP 2016504239 A JP2016504239 A JP 2016504239A JP 6855794 B2 JP6855794 B2 JP 6855794B2
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- Sustainable Development (AREA)
- Photovoltaic Devices (AREA)
Description
本発明における湿潤ゲルとは、液体を保有しているゲルであり、具体的には固体の分散質と液体の分散媒を含み、分散質の最小構成単位が物理相互作用により形成された三次元的なネットワークを形成し、そのネットワーク中に分散媒が取り込まれたゲルである。スクリーン印刷などにおいて十分な印刷性を得るためには、高剪断時と低剪断時の粘度に大きな差、すなわちチクソトロピー性が必要である。本発明の湿潤ゲルにおいては、ファンデルワールス力などの比較的弱い物理相互作用を用いることにより、剪断などの外力により一部または全部の相互作用が切断され、流動性が生じ、外力が作用しない時には流動性が生じないため、十分なチクソトロピー性が得られる。
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。
次に、図4(c)に示すように、p型不純物拡散組成物4とn型不純物拡散組成物2を半導体基板1中に同時に拡散させ、p型不純物拡散層5とn型不純物拡散層3を形成する。不純物拡散組成物の塗布方法、焼成方法および拡散方法としては前記と同様の方法が挙げられる。
MMB:3−メトキシ−3−メチル−1−ブタノール。
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5rpm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5rpmでの測定値を粘度とし、回転数50rpmでの測定値(η50)と回転数5rpmでの測定値(η5)の比(η5/η50)をチクソ性とした。
不純物拡散組成物を孔径0.1μmのPTFEメンブレンフィルターを用いて、圧力空気(0.1MPa)にて加圧ろ過した。フィルター上に残存した固形物をデジタルマイクロスコープVHX−1000((株)キーエンス製)で観察し、画像解析を用いてゲル50個の投影面積を測定後、該投影面積と同じ面積の円の直径を算出し、それらの平均値を湿潤ゲルサイズとした。
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℃で5分間処理した。
シート抵抗値測定に用いた拡散後のシリコンウェハーに対して、二次イオン質量分析装置IMS7f(Camera社製)を用いて、不純物の表面濃度分布を測定した。得られた表面濃度分布から100μm間隔で10点の表面濃度を読み取り、その平均と標準偏差の比である「標準偏差/平均」を計算し、「標準偏差/平均」が0.3以下のものをexcellent(A)、0.3を上回り0.6以下のものをgood(B)、0.6を上回り1.0以内のものをfair(C)、1.0を上回るものをbad(D)と判定した。
(1)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Aの固形分濃度は39.8重量%であった。
500mLの三口フラスコに分散媒としてテルピネオール450g、分散質としてアエロジルRY200S(日本アエロジル(株)製、数平均粒子径16nm)50gを加え、室温で1時間攪拌した。得られた溶液を三本ロールミルEXAKT M−50I((株)永瀬スクリーン印刷研究所製)に注入し、ローラー速度比3.3:1.8:1の条件で4回通過させて分散し、湿潤ゲル溶液Aを得た。
上記で合成したポリシロキサン溶液94g、上記で調整した湿潤ゲル溶液A103g、リン酸34g、増粘剤としてPEO−1(酸化ポリエチレン系増粘剤、住友精化(株)製)30g、γ−ブチロラクトン189g、純水50gを混合し、均一になるように十分撹拌して、不純物拡散組成物Aを得た。
三本ロールミルを通過させる回数を2回としたこと以外は実施例1と同様にして不純物拡散組成物Bを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、いずれも良好であった。
三本ロールミルの代わりにDYNO−MILL KD−6((株)シンマルエンタープライゼス製)を用いたこと以外は実施例1と同様にして不純物拡散組成物Cを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、いずれも良好であった。
増粘剤としてPEO−1の代わりにKC−7000(アクリル系増粘剤、共栄社化学(株)製)を用いたこと以外は実施例3と同様にして不純物拡散組成物Dを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、いずれも良好であった。
増粘剤としてPEO−1の代わりにエトセル100cP(セルロース誘導体、ダウケミカル製)を用いたこと以外は実施例3と同様にして不純物拡散組成物Eを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、いずれも良好であった。
500mLの三口フラスコに分散媒としてMMB450g、分散質としてフローノンEC121(共栄社化学(株)製)50gを加え、室温で1時間攪拌した。得られた溶液を三本ロールミルEXAKT M−50I((株)永瀬スクリーン印刷研究所製)に注入し、ローラー速度比3.3:1.8:1の条件で4回通過させて分散し、湿潤ゲル溶液Bを得た。次にポリシロキサン溶液94g、上記で調整した湿潤ゲル溶液B50g、リン酸34g、PEO−1(住友精化(株)製)30g、γ−ブチロラクトン242g、純水50gを混合し、均一になるように十分撹拌して、不純物拡散組成物Fを得た。
n型不純物拡散層およびp型不純物拡散層形成方法
図5(a)に示すように、n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、n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6(a)に示すように、n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、n型シリコンウェハー61を100℃5分間プリベークした。
三本ロールミルでの分散を実施しなかったこと以外は実施例1と同様に不純物拡散組成物Gを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、パターン精度、拡散均一性に劣る結果であった。
三本ロールミルの代わりにプラネタリーミキサーを用いたこと以外は実施例1と同様にして不純物拡散組成物Hを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、パターン精度、拡散均一性に劣る結果であった。
三本ロールミルの代わりに自転・公転ミキサー(シンキー製AR−100)を用いたこと以外は実施例1と同様にして不純物拡散組成物Iを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、パターン精度、拡散均一性に劣る結果であった。
三本ロールミルの代わりにローラーミルRM−005M(浅田鉄工(株)製)を用いたこと以外は実施例1と同様にして不純物拡散組成物Jを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、パターン精度、拡散均一性に劣る結果であった。
湿潤ゲルを用いなかったこと以外は実施例1と同様に不純物拡散組成物Kを得た。パターン精度、シート抵抗値、拡散均一性を測定したところ、表2に示すとおり、パターン精度が大きく劣る結果であった。
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
51 n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 n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 (7)
- (A)(a1)数平均粒子径が10nm以上30nm以下である酸化ケイ素の粒子と、(a2)液体の分散媒としてのテルピネオール、とを含み、サイズが1μm以上30μm以下である湿潤ゲルと、(B)不純物拡散成分と、(C)下記一般式(1)で表されるポリシロキサンと、(D)増粘剤と、を含有する不純物拡散組成物。
- 回転数50rpmでの粘度(η50)と回転数5rpmでの粘度(η5)との比(η5/η50)が1.5以上5.0未満である請求項1記載の不純物拡散組成物。
- 前記(D)増粘剤がセルロース誘導体を含む請求項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。
- 前記印刷がスクリーン印刷である請求項4記載の半導体素子の製造方法。
- 前記不純物拡散組成物膜をマスク層として、前記不純物とは異なる第2の不純物を含む不純物拡散組成物を印刷して第2の不純物拡散組成物膜を形成する工程を含む請求項4または5記載の半導体素子の製造方法。
- 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第1の不純物拡散組成物膜を形成する工程と、第2の不純物を含む不純物拡散組成物を印刷して第2の不純物拡散組成物膜を形成する工程と、前記第1の不純物拡散組成物膜と前記第2の不純物拡散組成物膜を同時に加熱することにより第1の不純物拡散層と第2の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。
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