JP2010514563A - 金属アルコキシド含有フィルムの硬化方法 - Google Patents
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- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/08—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by flames
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- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/54—Apparatus specially adapted for continuous coating
- C23C16/545—Apparatus specially adapted for continuous coating for coating elongated substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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Abstract
Description
本出願は2006年12月29日出願の米国特許仮出願第60/882,625号の優先権を主張するものである。
本発明は、薄い、無機又はハイブリッド無機/有機フィルムの製造方法に関する。
トリメトキシシラン官能基によって両端が官能化された、下記一般式:
X−CF2O(CF2O)m(C2F4O)cCF2−X
[式中、X=CONHCH2CH2CH2Si(OCH3)3であり、mは約10であり、nは約10である]にて示される、平均分子量約2000のフッ素化ポリエーテルオリゴマーによって、30.5×22.9cm(12×9インチ)で厚さ0.95cm(0.375インチ)のポリカーボネートプレートをコーティングした。このフッ素化トリアルコキシシランポリエーテルオリゴマーを、米国特許第6,045,864号及び図2に記載されるような方法によって霧化して蒸発させた。噴霧器への液体の流速は0.075ml/分であった。噴霧器への高温の窒素流は186℃で44lpmであった。蒸発器領域の温度は162℃であった。基材を拡散器から流出する蒸気流に5秒間曝露することによって、ポリカーボネートプレート上に極めて薄い、凝縮液体コーティングを形成した。
実施例1の手順を用いてフッ素化トリアルコキシシランポリエーテルオリゴマーからなる同様のコーティングを調製した。このコーティングを対流エアオーブン内で5〜60分間、130〜140℃で硬化させて硬化反応を終了させた。飛行時間型2次イオン質量分析(TOFSIMS)の結果は、触媒バーナーからのガス状生成物への1秒間の曝露により、130℃のオーブンで1時間硬化させた場合に一般に見られるのと同程度にコーティングが完全に硬化したことを示すものであった。
ここでもやはり、触媒燃焼ヒーターの生成物へ曝露することによって硬化させたフッ素化トリアルコキシシランポリエーテルオリゴマーのコーティングを、直径7.6cm(3インチ)のシリコンウェーハ、ガラスウェーハ、二軸延伸ポリプロピレン(BOPP)基材、及び二軸延伸ポリ(エチレンテレフタレート)基材上に形成した。触媒ヒーターによって高い硬化度が与えられ、硬化した材料には撥液性が認められた。
実施例1の手順を用いて、30.5cm×22.9cm(12インチ×9インチ)のポリカーボネートプレートにフッ素化トリアルコキシシランポリエーテルオリゴマーをコーティングした。ただし以下の変更を行った。すなわち、拡散器を幅25.4cm(10インチ)のスロットコーティングダイに置き換え、液体モノマーの流速を0.10ml/分とし、噴霧器への窒素流を300℃で50 lpmとし、蒸発領域の温度を300℃とし、基材は2.54cm/秒(1インチ/秒)でコーティングダイスロットを通過させた。液体コーティングは触媒燃焼源からの高温の水蒸気流に曝すことによって硬化させた。30.5×10.2cm(12×4インチ)の触媒バーナー(フリン・バーナー(Flynn Burner Corp.)社)は、10.9kL/時(385ft3/時)の乾燥した、埃を濾過した空気と、1.1kL/時(40ft3/時)の天然ガスからなる可燃性混合物によって支持され、40,000Btu/時・インチの火力を得た。火炎当量比は1.00であった。触媒バーナーとコーティングされた基材との間の間隙は約5.1cm(2インチ)であった。曝した時間は2秒未満であった。硬化後、コーティングは溶媒ベースのインクを弾いた。
Claims (26)
- 基材に金属アルコキシド層を適用する工程と、該金属アルコキシド層を水の存在下で触媒燃焼バーナーからの熱に曝露することによって該層を硬化させる工程と、を含む基材上に無機又はハイブリッド有機/無機層を形成する方法。
- 前記触媒燃焼ヒーターが水を与える、請求項1に記載の方法。
- 前記アルコキシド層を適用する工程が、蒸発した金属アルコキシドを凝縮させて前記基材上に層を形成させることを含む、請求項1又は2に記載の方法。
- 前記金属アルコキシドが、アルミニウム、アンチモン、ヒ素、バリウム、ビスマス、ホウ素、セリウム、ガドリニウム、ガリウム、ゲルマニウム、ハフニウム、インジウム、鉄、ランタン、リチウム、マグネシウム、モリブデン、ネオジム、リン、ケイ素、ナトリウム、ストロンチウム、タンタル、タリウム、スズ、チタン、タングステン、バナジウム、イットリウム、亜鉛、及びジルコニウムのアルコキシド、又はこれらの混合物を含む、請求項1〜3のいずれか一項に記載の方法。
- 前記金属アルコキシドが、チタン、ジルコニウム、ケイ素、アルミニウム、タンタル、バリウム、スズ、インジウム、亜鉛、ガリウム、ビスマス、マグネシウム、ストロンチウム、ホウ素、セリウム、ハフニウム、ネオジム、ランタン、タングステンのアルコキシド、又はこれらの混合物を含む、請求項4に記載の方法。
- 前記金属アルコキシドが、テトラ(エトキシ)チタネート、テトラ(イソプロポキシ)チタネート、テトラ(n−プロポキシ)チタネート、ポリジメトキシシロキサン、メチルトリアセトキシシラン、テトラ(n−プロピル)ジルコネート、テトラ(n−ブトキシ)ジルコネート、又はこれらの混合物を含む、請求項5に記載の方法。
- 前記金属アルコキシドがトリアルコキシシランを含む、請求項4に記載の方法。
- 前記金属アルコキシドが少なくとも2種類のアルコキシドの混合物を含み、そして前記アルコキシドの割合が前記無機又はハイブリッド有機/無機層に所定の屈折率を提供するように選択される、請求項4に記載の方法。
- 前記金属アルコキシドが少なくとも2種類のアルコキシドの混合物を含み、そして前記アルコキシドの割合が前記無機又はハイブリッド有機/無機層に所定の硬度を提供するように選択される、請求項4に記載の方法。
- 前記層を約0.1秒から約10秒間加熱することを含む、請求項1〜9のいずれか一項に記載の方法。
- 前記層を約0.3秒から約5秒間加熱することを含む、請求項10に記載の方法。
- 前記層を約0.5秒から約2秒間加熱することを含む、請求項11に記載の方法。
- 前記基材がポリマー、金属、ガラス、セラミック、複合材、紙又は木材である、請求項1〜12のいずれか一項に記載の方法。
- 前記基材がポリマーである、請求項13に記載の方法。
- 前記ポリマーがポリエステルである、請求項14に記載の方法。
- 前記ポリエステルがポリ(エチレンテレフタレート)である、請求項15に記載の方法。
- 金属アルコキシド及び有機化合物を適用して基材上に層を形成させる工程と、
前記層を水の存在下で触媒燃焼ヒーターからの熱に曝露することによって該層を硬化させる工程と、を含む、基材上にハイブリッド有機/無機層を形成する方法。 - 前記金属アルコキシドと有機化合物の層を適用する工程は、蒸発した金属アルコキシドと蒸発した有機化合物との混合物を凝縮させることによって前記基材上に層を形成させることを含む、請求項17に記載の方法。
- 前記蒸発したアルコキシドと前記蒸発した有機化合物とが別々に蒸発させられ、前記基材上に凝縮される前に蒸気相中で混合される、請求項18に記載の方法。
- 前記アルコキシドと前記有機化合物とが同時に蒸発させられる、請求項18に記載の方法。
- 前記アルコキシド及び前記有機化合物とが、フラッシュ蒸発法を使用して蒸発させられる、請求項17〜20のいずれか一項に記載の方法。
- 前記層を約0.1秒〜約10秒間加熱することを含む、請求項17〜21のいずれか一項に記載の方法。
- 前記層を約0.3秒〜約5秒間加熱することを含む、請求項22に記載の方法。
- 前記層を約0.5秒〜約2秒間加熱することを含む、請求項23に記載の方法。
- 前記有機化合物がアルコール、カルボン酸、エステル、酸無水物、アセチルハロゲン、チオール、又はアミンを含む、請求項17〜24のいずれか一項に記載の方法。
- 前記エステルがアクリレートを含む、請求項25に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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US88262506P | 2006-12-29 | 2006-12-29 | |
US60/882,625 | 2006-12-29 | ||
PCT/US2007/089098 WO2008083310A1 (en) | 2006-12-29 | 2007-12-28 | Method of curing metal alkoxide-containing films |
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JP2010514563A true JP2010514563A (ja) | 2010-05-06 |
JP2010514563A5 JP2010514563A5 (ja) | 2011-02-10 |
JP5249240B2 JP5249240B2 (ja) | 2013-07-31 |
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US (1) | US8227040B2 (ja) |
EP (1) | EP2118336B1 (ja) |
JP (1) | JP5249240B2 (ja) |
KR (1) | KR101529332B1 (ja) |
CN (1) | CN101573471A (ja) |
BR (1) | BRPI0721301A2 (ja) |
WO (1) | WO2008083310A1 (ja) |
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WO2010002755A2 (en) | 2008-06-30 | 2010-01-07 | 3M Innovative Properties Company | Method of making inorganic or inorganic/organic hybrid barrier films |
US20100081009A1 (en) * | 2008-09-26 | 2010-04-01 | General Electric Company | Spray Application of Liquid Precursors for CMAS Resistant Coatings |
DE102009028801B3 (de) | 2009-08-21 | 2011-04-14 | Evonik Degussa Gmbh | Verfahren zur Herstellung Indiumoxid-haltiger Schichten, nach dem Verfahren herstellbare Indiumoxid-haltige Schicht und deren Verwendung |
DE102009028802B3 (de) * | 2009-08-21 | 2011-03-24 | Evonik Degussa Gmbh | Verfahren zur Herstellung Metalloxid-haltiger Schichten, nach dem Verfahren herstellbare Metalloxid-haltige Schicht und deren Verwendung |
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DE102010031592A1 (de) | 2010-07-21 | 2012-01-26 | Evonik Degussa Gmbh | Indiumoxoalkoxide für die Herstellung Indiumoxid-haltiger Schichten |
DE102010031895A1 (de) | 2010-07-21 | 2012-01-26 | Evonik Degussa Gmbh | Indiumoxoalkoxide für die Herstellung Indiumoxid-haltiger Schichten |
DE102010043668B4 (de) | 2010-11-10 | 2012-06-21 | Evonik Degussa Gmbh | Verfahren zur Herstellung von Indiumoxid-haltigen Schichten, nach dem Verfahren hergestellte Indiumoxid-haltige Schichten und ihre Verwendung |
ES2700519T3 (es) * | 2011-05-06 | 2019-02-18 | Tesa Se | Procedimiento para el aumento de las propiedades adhesivas de masas adhesivas sensibles a la presión sobre sustratos por medio de tratamiento por plasma |
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WO2013022669A2 (en) | 2011-08-05 | 2013-02-14 | 3M Innovative Properties Company | Systems and methods for processing vapor |
TW201343817A (zh) * | 2012-02-28 | 2013-11-01 | Daikin Ind Ltd | 具有含氟矽烷系塗膜之物品的製造方法 |
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ITRM20120291A1 (it) * | 2012-06-21 | 2013-12-22 | Agenzia Naz Per Le Nuove Tecn Ologie L Ener | Metodo per il trattamento di superfici metalliche per conferire alle stesse una elevata idrofobicita' ed oleofobicita' |
US9404002B2 (en) * | 2014-02-06 | 2016-08-02 | Transtron Solutions Llc | Molecular precursor compounds for indium gallium zinc oxide materials |
US9670232B2 (en) * | 2014-02-06 | 2017-06-06 | Transtron Solutions Llc | Molecular precursor compounds for zinc-group 13 mixed oxide materials |
CN106319466A (zh) * | 2016-10-12 | 2017-01-11 | 东北林业大学 | 在竹材表面仿生制备高粘附超疏水的方法 |
EP3409813A1 (en) | 2017-06-01 | 2018-12-05 | Evonik Degussa GmbH | Device containing metal oxide-containing layers |
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CN111936667B (zh) * | 2018-03-30 | 2022-12-13 | 大金工业株式会社 | 叠层体的制造方法 |
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- 2007-12-28 WO PCT/US2007/089098 patent/WO2008083310A1/en active Application Filing
- 2007-12-28 CN CNA2007800486713A patent/CN101573471A/zh active Pending
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CN101573471A (zh) | 2009-11-04 |
US20100068382A1 (en) | 2010-03-18 |
KR101529332B1 (ko) | 2015-06-16 |
US8227040B2 (en) | 2012-07-24 |
JP5249240B2 (ja) | 2013-07-31 |
BRPI0721301A2 (pt) | 2014-03-25 |
KR20090101201A (ko) | 2009-09-24 |
WO2008083310A1 (en) | 2008-07-10 |
EP2118336B1 (en) | 2017-02-15 |
EP2118336A1 (en) | 2009-11-18 |
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