JP4928940B2 - 酸化層により接着される多層コーティングの制御された気相堆積 - Google Patents
酸化層により接着される多層コーティングの制御された気相堆積 Download PDFInfo
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- 125000003808 silyl group Chemical group [H][Si]([H])([H])[*] 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 description 1
- QHAHOIWVGZZELU-UHFFFAOYSA-N trichloro(trichlorosilyloxy)silane Chemical compound Cl[Si](Cl)(Cl)O[Si](Cl)(Cl)Cl QHAHOIWVGZZELU-UHFFFAOYSA-N 0.000 description 1
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
Classifications
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Description
[0080]図1は、薄コーティングの気相堆積用装置100の概略的な断面図を示す。装置100は、薄い(典型的には0.5nm〜50nmの厚さ)コーティングが内部で気相堆積される処理チャンバ102を備える。コーティングされるべき基板106は、温度制御された基板ホルダ104、典型的には、基板ホルダ104の凹み107内に配置される。
[0090]本発明の方法は、前述の処理チャンバ又は同種の処理チャンバが使用されるコーティングの気相堆積を提供する。各コーティング前駆物質は、前駆物質の蒸気が蓄積される前駆物質蒸気リゾルバに、蒸気の形態で移動される。コーティング層の堆積に必要な量である公称の量の前駆物質蒸気が、前駆物質蒸気リゾルバに蓄積される。少なくとも一つのコーティング前駆物質は、コーティングされるべき基板が配置される処理チャンバに、前駆物質蒸気リゾルバからチャージされる。ある場合には、少なくとも一つの触媒蒸気が少なくとも一つの前駆物質蒸気に加えて処理チャンバに追加され、この際、触媒と前駆物質の蒸気の相対的な量は、コーティングによって示されるべき物理的特性に基づいている。ある場合では、少なくとも一つの前駆物質蒸気(及び任意の触媒蒸気)に加えて、希釈ガスが処理チャンバに追加される。希釈ガスは化学的に不活性で所望の処理圧力の合計を増加するために使用される一方で、コーティングの前駆物質及び任意の触媒成分の分圧の量は様々である。
[0098]酸化物層の表面上で得られる制御された数のOH反応点を有する酸化ケイ素層の堆積
[0099]基板表面の疎水性/親水性を(例えば、表面が疎水性から親水性に、又は親水性表面がより親水性になるよう)調節する技術は、基板の表面上に得られるOH反応点の数を調節するものとして考えられる。このような技術の一つは、酸化物表面上で得られる所望の濃度のOH反応点を提供しながら基板表面上に酸化物コーティングを形成することである。図2に、酸化物形成のメカニズムの概略図200を示す。特に、基板202は、基板表面203にOH基204を有する。図示するテトラクロロシランのようなクロロシラン208と水206は、OH基204と同時に又は順に反応して基板202の表面203に示される酸化物層208及び副産物HCl210を生成する。更に、クロロシラン前駆物質、クロロシロキサン、フルオロシラン、及びフルオロシロキサンが使用されてもよい。
[0102]以下に説明する好ましい実施形態(実施例)では、酸化ケイ素コーティングがガラス基板上に形成された。ガラス基板は、処理チャンバ中(チャンバが約20ミリトルにポンプダウンされた後)の残留水分のなかで酸素プラズマによって処理され、清潔な表面(有機汚染物質がない)が得られ、ガラス表面に最初のOH基が形成された。
[0116]酸化物形成シラン及び官能基を含む有機シランが同時に堆積(共堆積)されると、処理チャンバへの一連の前駆物質の追加が重要となるほど反応が早くなる。例えば、SiCl4/FOTS/H2Oの共堆積処理において、FOTSが最初に導入されると、島の形態で極めて迅速にガラス基板表面に堆積され、同質の合成膜の堆積が防止される。この例は、以下の表IIIに示される。
[0132]図3A及び3Bは、シリコン基板上に形成される酸化ケイ素結合層の表面の原子間力顕微鏡(AFM)画像の概略図を示す。初期のシリコン基板表面のRMS粗さは約0.1nm未満と決定される。図3Aは、基板がシリコンであった場合の堆積処理を示す。シリコンの表面は、表面を洗浄してシリコン表面にヒドロキシルを形成できるようにするために、本明細書で前述した方法で酸素プラズマに曝される。SiCl4蒸気リザルバから処理チャンバにSiCl4がチャージされ、コーティング処理チャンバで0.8トルの分圧が作られた。10秒以内にH2O蒸気リゾルバから処理チャンバにH2O蒸気がチャージされ、コーティング処理チャンバで4トルの分圧が作られた。コーティング処理チャンバにおける合計圧力は4.8トルとなった。基板温度及び処理チャンバ壁の温度は、約35℃であった。基板は、SiCl4とH2Oの混合物に10分間曝された。得られた酸化ケイ素コーティングの厚さは約3nmであった。RMSでのコーティング粗さは1.4nmであり、Raは0.94nmであった。
[0135]図4は、DDMS(ジメチルジクロロシラン)前駆物質から生成される有機シランコーティングとの基板露出時間(反応時間)に相関するものとして水接触角(表面の疎水性の表示)の依存関係のグラフ400を示す。シリコン基板は、本明細書で前述したような酸素プラズマ処理によって表面ヒドロキシル基を提供するために洗浄され、機能的にされる。DDMSは1トルの分圧で適用され、10秒以内にH2Oが2トルの分圧で適用され、3トルの処理チャンバ内の合計圧力が生成される。
[0138][実施形態6]
[0139]図6Aは、酸化ケイ素コーティングの堆積中に処理チャンバに存在する四塩化ケイ素の分圧及び水蒸気の分圧に相関するものとしてシリコン表面に堆積される酸化ケイ素結合層の膜厚さの三次元図600であり、基板及びコーティング処理チャンバ壁の温度は約35℃であり、コーティング前駆物質にシリコン基板が曝される時間は全ての前駆物質材料の追加が完了した4分後であった。最初に前駆物質SiCl4蒸気が処理チャンバに追加され、10秒後に前駆物質H2O蒸気が追加された。コーティング処理チャンバにおけるH2Oの分圧は、軸602に示され、SiCl4の分圧は軸604に示される。膜厚さは、オングストロームで軸606に示される。前駆物質の追加後の膜堆積時間は4分であった。より薄いコーティングは、より平坦な表面を示し、グラフ600上の点608におけるコーティングのRMS粗さは1nm(10A)の範囲であった。より厚いコーティングはより粗い表面を示したが、当分野において一般的に公知のコーティングよりはまだ平坦であった。グラフ600の点610において、コーティングのRMS粗さは4nm(40A)の範囲であった。
[0169]複数の酸化物層及び複数の有機物層を備える多層コーティングの一つの適用例は、印刷に一般的に用いられるインクジェットである。精細な文字サイズを印刷する性能は、印刷されるべき表面に到達する前にインクが流れる開口部の大きさに依存する。更に、使用されるインクによっては、開口部の表面上でのインクの容易な流れ及び所望のジェット動作を得るために、表面が本質的に親水性又は疎水性である必要があり、インクと開口部の表面との間の様々な度合いの接触角が効果をもたらすために利用される。
Claims (37)
- コーティングが特定の特性を示すように調整される、基板上に多層コーティングを堆積する方法であって、
前記多層コーティングの全ての層が気相から堆積され、
前記多層コーティングは、少なくとも1つの酸化物層、及び、ペルフルオロデシルトリクロロシラン(FDTS)、ウンデセニルトリクロロシラン(UTS)、デシルトリクロロシラン(DTS)、オクタデシルトリクロロシラン(OTS)、ジメチルジクロロシラン(DDMS)、ドデセニルトリクロロシラン(DDTS)、フルオロ−テトラヒドロオクチルジメチルクロロシラン(FOTS)、ペルフルオロオクチルジメチルクロロシラン、及び、ペルフルオロデシルジメチルクロロシランからなる群から選択された前駆物質が堆積された、最終表面層となる少なくとも1つの有機物層を含み、
前記気相からの前記堆積では、前記多層コーティングの少なくとも一層又は少なくとも一層の一部分の形成中に、反応基の停滞源が用いられ、
前記反応基の前記停滞源の正確な量の前駆物質試薬は、処理チャンバにチャージされ、前記少なくとも一層又は前記少なくとも一層の一部分の形成中に更に追加されることはない、方法。 - 複数の酸化物層が堆積される、請求項1記載の方法。
- 少なくとも1つの追加の堆積ステップにおいて、堆積のための前駆物質種を供給するよう非反応性キャリアガスを用いる、請求項2記載の方法。
- 前記気相堆積において、前記多層コーティングの各層の形成中に反応基の停滞源を用い、
前記反応基の前記停滞源は、前記処理チャンバにチャージされ、各層の形成中に更に追加されることはない、請求項1記載の方法。 - 前記多層コーティングの最終表面層ではない酸化物層それぞれの堆積後に、プラズマ処理が行われる、請求項1記載の方法。
- 前記複数の酸化物層及び有機物層は、酸化物層が有機物層と交互に配置されるように堆積される、請求項1記載の方法。
- 基板上に第1の有機物層を堆積する前に、酸化物層が前記基板上に形成される、請求項1記載の方法。
- 前記酸化物層の露出された表面が−OH基を含む、請求項7記載の方法。
- 前記酸化物層の露出された表面がハロゲン基を含む、請求項7記載の方法。
- 前記ハロゲン基が塩素を含む、請求項9記載の方法。
- 前記酸化物層の堆積前に、前記基板が酸素ベースプラズマを用いて処理される、請求項7記載の方法。
- 複数の酸化物層の厚さの合計は、前記多層コーティングの厚さの50%よりも大きい、請求項1記載の方法。
- 前記酸化物層の酸化物は、クロロシラン蒸気と水蒸気との反応によって形成される、請求項7記載の方法。
- 前記クロロシラン蒸気と前記水蒸気とは、前記基板の表面上で反応する、請求項13記載の方法。
- 前記クロロシラン蒸気と前記水蒸気との間の前記反応を制御するために、クロロシラン蒸気の分圧と水蒸気の分圧の組み合わせが用いられる、請求項13記載の方法。
- 前記クロロシランは、テトラクロロシラン、ヘキサクロロシラン及びその組み合わせからなる群から選択される、請求項15記載の方法。
- 前記処理チャンバにおける合計圧力が0.5トル〜400トルの範囲にあり、前記クロロシラン蒸気の分圧が0.5トル〜100トルの範囲にある、請求項15記載の方法。
- 前記酸化物の堆積中の基板温度は、10℃〜130℃の範囲にある、請求項17記載の方法。
- 前記処理チャンバの内壁の温度は、20℃〜150℃の範囲にある、請求項18記載の方法。
- 前記水蒸気の分圧は、0.5トル〜300トルの範囲にある、請求項15記載の方法。
- 前記酸化物表面に対する前記酸化物の堆積及びヒドロキシル基の生成後、特定の官能基を含む有機クロロシラン蒸気が前記ヒドロキシル基と反応して、特定の官能性特徴を前記多層コーティングに与える、請求項15記載の方法。
- 前記反応が前記基板表面上で行われるよう、前記有機クロロシラン蒸気と前記ヒドロキシル基との前記反応を制御するために、前記有機クロロシラン蒸気の分圧が使用される、請求項21記載の方法。
- 前記反応は、前記基板表面上で行われる、請求項22記載の方法。
- 前記有機クロロシラン蒸気は、アルキル基、アルコキシル基、フッ素含有アルキル置換基、フッ素含有アルコキシル置換基、ビニル基、エチニル基、エポキシ基、グルコキシ基、アクリル基、シリコン原子又は酸素原子含有グリコール置換基、アミノ基、及びその組み合わせからなる群から選択される官能基を含む、請求項21記載の方法。
- 前記処理チャンバにおける合計圧力が0.5トル〜30トルの範囲にあり、前記有機クロロシラン蒸気の分圧が0.1トル〜20トルの範囲にある、請求項24記載の方法。
- 前記有機クロロシラン蒸気の堆積中の基板温度は、10℃〜130℃の範囲にある、請求項25記載の方法。
- 前記処理チャンバの内壁の前記温度は、20℃〜150℃である、請求項26記載の方法。
- 多層コーティングの前記層が堆積される処理チャンバにおける合計圧力、少なくとも一つの前駆物質の分圧、前記多層コーティングの前記層が堆積される基板の温度、及び、前記処理チャンバの内壁の少なくとも1つの温度を制御することによって、各層の堆積速度、又は、個々の層を形成するために用いられる一連の段階における少なくとも1つの段階の堆積速度が制御される、請求項1記載の方法。
- 前記多層コーティングの前記層が堆積される処理チャンバにおける合計圧力、少なくとも1つの前駆物質の分圧、前記多層コーティングの前記層が堆積される基板の温度、及び、前記処理チャンバの内壁の少なくとも1つの温度を調整することによって、各層の堆積速度又は個々の層を形成するために用いられる一連の段階における各堆積段階、及び、前記多層コーティングの表面粗さが制御される、請求項1記載の方法。
- 前記多層コーティングが気相から堆積され、
少なくとも1つの層が、前記多層コーティングが内部で堆積されるコーティング堆積チャンバに導入される有機シラン前駆物質を用いて形成され、
少なくとも1つの層の表面粗さが、前記堆積チャンバにおける合計圧力、少なくとも一つの前駆物質の分圧、及び、前記コーティングが堆積される基板の温度を調整することで更に制御される、請求項1記載の方法。 - 少なくとも2つの有機シラン前駆物質が前記コーティング堆積チャンバに導入され、続いて、水が導入されることで前記有機シラン前駆物質の制御可能な共堆積が得られる、請求項30記載の方法。
- 各前駆物質の分圧は、前記コーティングの前記堆積速度又は前記表面粗さを調節するよう制御される、請求項30記載の方法。
- 前記水の前駆物質の分圧は、前記コーティングの前記堆積速度又は前記表面粗さを調節するよう制御される、請求項31記載の方法。
- 前記基板と直接的に接触する酸化物層の厚さは、前記基板の化学組成に相関するものとして制御され、
SAM有機物層は、前記酸化物層上に直接的に堆積され、
これにより、前記SAM有機物層の前記酸化物層と結合する能力が、前記酸化物層の表面被覆率及び厚さを制御することで向上される、請求項1記載の方法。 - 少なくとも2つの酸化物層と少なくとも1つの有機物層の堆積を含む請求項1記載の方法であって、それぞれの層が気相から堆積され、
前記酸化物層と前記有機物層は交互に配置され、
酸化物層が前記基板の表面上に直接的に堆積される、請求項1記載の方法。 - 前記多層コーティングが少なくとも2つの酸化物層と少なくとも2つの有機物層を含む、請求項35記載の方法。
- 前記多層コーティングが少なくとも5つの酸化物層と少なくとも5つの有機物層を含む、請求項36記載の方法。
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US10/862,047 US7638167B2 (en) | 2004-06-04 | 2004-06-04 | Controlled deposition of silicon-containing coatings adhered by an oxide layer |
US10/862,047 | 2004-06-04 | ||
US10/996,520 US20050271893A1 (en) | 2004-06-04 | 2004-11-23 | Controlled vapor deposition of multilayered coatings adhered by an oxide layer |
US10/996,520 | 2004-11-23 | ||
US11/112,664 US7776396B2 (en) | 2004-06-04 | 2005-04-21 | Controlled vapor deposition of multilayered coatings adhered by an oxide layer |
US11/112,664 | 2005-04-21 | ||
PCT/US2005/018313 WO2005121397A2 (en) | 2004-06-04 | 2005-05-24 | Controlled vapor deposition of multilayered coatings adhered by an oxide layer |
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US10900123B2 (en) | 2003-06-27 | 2021-01-26 | Spts Technologies Limited | Apparatus and method for controlled application of reactive vapors to produce thin films and coatings |
JP2014196568A (ja) * | 2004-06-04 | 2014-10-16 | アプライド マイクロストラクチャーズ,インコーポレイテッド | 酸化層により接着される多層コーティングの制御された気相堆積 |
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US8298614B2 (en) | 2012-10-30 |
CN1878888A (zh) | 2006-12-13 |
JP2007505220A (ja) | 2007-03-08 |
TWI422702B (zh) | 2014-01-11 |
CN1878888B (zh) | 2010-10-27 |
US8545972B2 (en) | 2013-10-01 |
TW200726856A (en) | 2007-07-16 |
US20080081151A1 (en) | 2008-04-03 |
JP2010065320A (ja) | 2010-03-25 |
TW200604368A (en) | 2006-02-01 |
US20050271893A1 (en) | 2005-12-08 |
US20110052808A1 (en) | 2011-03-03 |
JP2014196568A (ja) | 2014-10-16 |
JP6254485B2 (ja) | 2017-12-27 |
US20100304132A1 (en) | 2010-12-02 |
US20050271900A1 (en) | 2005-12-08 |
US7776396B2 (en) | 2010-08-17 |
TWI366607B (en) | 2012-06-21 |
US20080026146A1 (en) | 2008-01-31 |
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