JP2014505783A - シリカの低温合成法 - Google Patents
シリカの低温合成法 Download PDFInfo
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- JP2014505783A JP2014505783A JP2013514337A JP2013514337A JP2014505783A JP 2014505783 A JP2014505783 A JP 2014505783A JP 2013514337 A JP2013514337 A JP 2013514337A JP 2013514337 A JP2013514337 A JP 2013514337A JP 2014505783 A JP2014505783 A JP 2014505783A
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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
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- 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
- C23C16/22—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 inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- 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
- B05D3/10—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 other chemical means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- 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
- B05D3/10—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 other chemical means
- B05D3/105—Intermediate treatments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- 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
- B05D3/10—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 other chemical means
- B05D3/107—Post-treatment of applied coatings
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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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45534—Use of auxiliary reactants other than used for contributing to the composition of the main film, e.g. catalysts, activators or scavengers
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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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
- C23C16/45548—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction
- C23C16/45551—Atomic layer deposition [ALD] characterized by the apparatus having arrangements for gas injection at different locations of the reactor for each ALD half-reaction for relative movement of the substrate and the gas injectors or half-reaction reactor compartments
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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
- C23C16/455—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 characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45595—Atmospheric CVD gas inlets with no enclosed reaction chamber
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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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Abstract
【選択図】図1
Description
本出願は、2010年6月8日に提出された米国特許出願第61/352,643号の出願日遡及の利益を主張し、その内容は、全体が参照により本明細書に組み込まれる。
本明細書において列挙されている全ての特許、特許出願および特許公開は、本明細書に記載されている発明の日現在において当業者に公知である技術の状態をより完全に記載するために、それらの全体が参照により本明細書に組み込まれる。
本発明は、海軍研究事務所によって認定された認可番号N00014−07−1−0690−DOD35CAPの下、および空軍科学研究局によって認定された認可番号FA9550−09−1−0669−DOD35CAPの下に合衆国政府支援によってなされた。合衆国政府は、この発明においてある種の権利を有する。
[技術の分野]
この技術は一般に、シリカまたはシリカ様薄膜に関する。特にこの技術は、シリカ薄膜の低温堆積に関する。
シリカの成長を、約5mLのTMOS(Sigma−Aldrich、98%)および約5mLの水酸化アンモニウム(Sigma−Aldrich、30重量%溶液)をそれぞれ含有する2個の25mLのガラス試験管(直径1cm)(図3)を用いて、ヒュームフード(fumehood)において実施した。基板サンプルを金属ワイヤに取り付け、以下に述べる時間の間、液面の上方およそ2cmのところに、各試験管内で交互に懸架した。結果として、基板サンプルをTMOSおよびNH3/H2O蒸気に順次暴露した。
TMOS/NH4OH暴露のサイクルを60℃で実施したことを除いて、実施例1と同様にポリカーボネートフィルムに堆積させた。図5のA及びCは、コーティングされていないポリカーボネートフィルムのエネルギー分散分光(EDS)スペクトルおよび走査電子顕微鏡(SEM)画像を示す。図5のB及びDは、シリカでコーティングされたポリカーボネートフィルムのEDSスペクトルおよびSEMを示す。示されているように、シリカは、ポリカーボネートフィルム表面上に容易に堆積する。
Claims (20)
- シリカフィルムを形成する方法であって、
周囲圧力および150℃未満の温度において有機基板をアルコキシシランの蒸気に暴露して、アルコキシシランが基板上に吸着されるようにする工程と、次いで、
周囲圧力において水蒸気および触媒に暴露することにより、吸着されたアルコキシシランをシリカに変換する工程と、
を含み、
前記アルコキシシランは、有機基板をアルコキシシランの蒸気に暴露する間、周囲圧力条件において水蒸気と実質的に反応しない、ことを特徴とする方法。 - 前記基板が温度感応性基板であり、基板の温度が、基板を不安定化、分解または溶融する温度より低い、請求項1に記載の方法。
- 前記基板がポリマー材料である、請求項1に記載の方法。
- 前記基板が生体材料である、請求項1に記載の方法。
- 前記アルコキシシランがテトラメトキシシランを含む、請求項1に記載の方法。
- 前記触媒がNH3を含む、請求項1に記載の方法。
- 前記アルコキシシラン蒸気が、アルコキシシラン源を加熱することによって得られる、請求項1に記載の方法。
- 前記アルコキシシラン源は100℃未満の温度に加熱される、請求項7に記載の方法。
- 前記アルコキシシラン蒸気が室温におけるものである、請求項1に記載の方法。
- 前記暴露工程および前記変換工程が繰り返される、請求項1に記載の方法。
- 前記暴露工程および前記変換工程が、10〜1000回の範囲で繰り返される、請求項8に記載の方法。
- 前記基板が、1秒〜120分の範囲の時間にわたってアルコキシシラン蒸気に暴露される、請求項1に記載の方法。
- 前記基板が、30秒〜60分の範囲の時間にわたって水蒸気に暴露される、請求項1に記載の方法。
- シリカ層を反応性酸素種に暴露する工程をさらに含む、請求項1に記載の方法。
- 前記基板がプラスチックフィルムである、請求項1に記載の方法。
- 前記プラスチックフィルムが、食品包装用途において用いられるプラスチックである、請求項15に記載の方法。
- 前記暴露工程および前記変換工程が、連続的なプラスチックフィルム生成プロセスの一部として実施される、請求項15に記載の方法。
- 前記暴露後、吸着されていないアルコキシシラン蒸気をパージする工程をさらに含む、請求項1に記載の方法。
- 前記変換後、吸着されていない水蒸気および触媒蒸気をパージする工程をさらに含む、請求項1に記載の方法。
- 前記基板が生体細胞である、請求項1に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US35264310P | 2010-06-08 | 2010-06-08 | |
US61/352,643 | 2010-06-08 | ||
PCT/US2011/039625 WO2011156484A2 (en) | 2010-06-08 | 2011-06-08 | Low-temperature synthesis of silica |
Publications (2)
Publication Number | Publication Date |
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JP2014505783A true JP2014505783A (ja) | 2014-03-06 |
JP5859521B2 JP5859521B2 (ja) | 2016-02-10 |
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Application Number | Title | Priority Date | Filing Date |
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JP2013514337A Expired - Fee Related JP5859521B2 (ja) | 2010-06-08 | 2011-06-08 | シリカの低温合成法 |
Country Status (7)
Country | Link |
---|---|
US (1) | US8993063B2 (ja) |
EP (1) | EP2580371A2 (ja) |
JP (1) | JP5859521B2 (ja) |
CN (1) | CN103025915B (ja) |
AU (1) | AU2011264922B2 (ja) |
CA (1) | CA2801912A1 (ja) |
WO (1) | WO2011156484A2 (ja) |
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JP2017531548A (ja) * | 2014-06-26 | 2017-10-26 | エーファウ・グループ・エー・タルナー・ゲーエムベーハー | 二酸化ケイ素層の施与方法 |
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US9765429B2 (en) | 2013-09-04 | 2017-09-19 | President And Fellows Of Harvard College | Growing films via sequential liquid/vapor phases |
US9953830B2 (en) * | 2014-03-13 | 2018-04-24 | Hitachi Kokusai Electric Inc. | Method of manufacturing semiconductor device, substrate processing apparatus and recording medium |
WO2016055865A1 (en) * | 2014-10-10 | 2016-04-14 | King Abdullah University Of Science And Technology | Oxide shell structures and methods of making oxide shell structures |
TW201823501A (zh) * | 2016-11-16 | 2018-07-01 | 美商陶氏全球科技有限責任公司 | 用於製造膜上之薄塗層之方法 |
KR102461975B1 (ko) * | 2020-10-29 | 2022-11-02 | 주식회사 비이아이랩 | 롤투롤 원자층 증착장치 |
JP2023090367A (ja) | 2021-12-17 | 2023-06-29 | エア・ウォーター株式会社 | 成膜方法 |
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CA2801912A1 (en) | 2011-12-15 |
WO2011156484A2 (en) | 2011-12-15 |
US20130236641A1 (en) | 2013-09-12 |
AU2011264922A1 (en) | 2013-01-10 |
WO2011156484A3 (en) | 2012-01-26 |
US8993063B2 (en) | 2015-03-31 |
CN103025915A (zh) | 2013-04-03 |
JP5859521B2 (ja) | 2016-02-10 |
AU2011264922B2 (en) | 2015-11-26 |
EP2580371A2 (en) | 2013-04-17 |
CN103025915B (zh) | 2015-08-05 |
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