JP4391944B2 - 反射比色センシング素子 - Google Patents
反射比色センシング素子 Download PDFInfo
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- JP4391944B2 JP4391944B2 JP2004541478A JP2004541478A JP4391944B2 JP 4391944 B2 JP4391944 B2 JP 4391944B2 JP 2004541478 A JP2004541478 A JP 2004541478A JP 2004541478 A JP2004541478 A JP 2004541478A JP 4391944 B2 JP4391944 B2 JP 4391944B2
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Description
「検体」とは、化学分析で検出の対象となる特定の成分を意味し;
「寸法変化」とは、検出層表面の表面に垂直な方向の距離の変化を意味し;
「多孔性材料」とは、その体積全体にわたり細孔の連続的網状構造を含有する材料を意味し;
「反射」とは、半反射または完全反射を意味し;
「半反射」とは、完全反射でも完全透過でもなく、好ましくは約30〜約70%、より好ましくは約40〜約60%の反射を意味し;
「実質的に連続な」とは、材料の層が非ポーラスであることを意味するが、亀裂、粒界、または材料の層を貫通する経路を形成する他の構造を有していてもよい。
基材はオプションであるが、存在する場合、比色センサーを支持することのできる任意の好適な材料を含みうる。それは可撓性であっても非可撓性であってもよい。基材材料は、用途に合わせることができる。好ましくは、真空堆積法で使用するのに好適である。
反射層は、完全反射層または半反射層を形成することのできる任意の材料を含みうる。材料は約20〜約200nmの厚さで完全反射性であることが好ましい。典型的には、より薄い層を使用して反射層を半反射性にすることができる。反射層は典型的には半反射層よりも反射性が高くなるように作製されるが、反射層と半反射層の反射率を同一にして検体の存在に対する応答をセンサーフィルムの両側から見えるようにすることが望ましい場合もある。
検出層は、1種以上のポリマーまたはコポリマーを含みうる。ほとんどの実施形態では、検出層は、検体に暴露されたときに光学的厚さが変化する少なくとも1種のポリマーを含む。光学的厚さの変化は、膨潤もしくは収縮によるポリマーの物理的厚さの変化のような寸法変化または検体の存在もしくは化学反応による検出層の屈折率変化により引き起こすことができる。検出層は、ある色から他の色へ、有色から無色へ、または無色から有色へ変化させうる。
半反射層は、浸透性で実質的に連続な半反射層を形成することができかつ検出層と異なる屈折率を有する任意の材料を含みうる。ほとんどの実施形態では、約5nmの厚さで半反射性であることが好ましい。なぜなら、この厚さであれば、ほとんどの検体がこの層に浸透して検出層に達することができるからである。所望の厚さは、層の形成に使用される材料、検出対象の検体、および検体を保有する媒体に依存するであろう。
追加の層がセンサーフィルムの光学素子を妨害しないかぎり、センサーフィルムは、先に記載した層のいずれかの間に追加の層を含みうる。追加の層は、タイ層、構造層などを含みうる。
本発明の多層フィルムは、米国特許第5,877,895号明細書中に記載されているような方法により作製することができる。また、検出層は、スピンコーティング法、溶液コーティング法、押出コーティング法、または当技術分野で公知の他の好適な方法により、作製可能である。プラズマ重合法のようなプラズマ堆積法により、検出層を作製することも可能である。また、反射層および半反射層は、蒸発法、スパッタリング法、化学気相堆積(CVD)法、プラズマ堆積法、または火炎堆積法のような標準的な蒸気コーティング法により作製可能である。反射層および半反射層を作製する他の方法は、溶液からめっきする方法である。
フィルムセンサーは、センサーと、光源と、場合により色の変化をセンサーによりモニターする手段と、を含む系で使用することも可能である。光源は、自然光源であっても人工光源であってもよい。モニタリングは、さまざまな方法で行うことが可能である。視覚的に、光ディテクターにより、または他の好適な手段により、行うことが可能である。
米国特許第5,877,895号明細書に記載されている堆積法により、多層比色センサーフィルムを作製した。
一連の溶媒蒸気に暴露する前および暴露した後に多層フィルムの可視反射スペクトルを測定した。フィルムセクション(実施例1の2.54平方cmのセクション)をガラススライド上に固定し、密封ジャー内で飽和有機蒸気に暴露した。平衡に達した後、暴露されたフィルムを取り出して、ただちにガラスカバースライドで覆い、蒸気脱着を防止した。その後、拡散反射UV−VIS分光計を用いて、暴露された材料の反射スペクトルを測定した。試験したすべての有機蒸気で、検体への暴露時に反射極大の実質的なレッドシフトが観察された。たとえば、524nm(暴露前)を中心とする反射極大は、長波長側へのシフト(レッドシフト)を呈する。表2に示されるように、シフトの大きさは、22nm(アセトニトリル)〜116nm(メチレンクロリド)の範囲であった。この実施例は、多層比色センサーフィルムが有機蒸気に応答して、ハロカーボン類、アレーン類、アルコール類、ケトン類、ニトリル類、およびエーテル類に対して比色シフトを呈することを示している。飽和水蒸気に暴露したときには反射スペクトル中にシフトは観察されなかった。液体の水の中にフィルムを沈めたときでさえも、色変化は観察されなかった。
さまざまな検体蒸気への応答感度を測定するために、実施例1に記載されているように作製したセンサーフィルムを簡単なフロースルー型装置により一連の濃度の検体に暴露した。濃度(分圧により決定した)を浴温により制御した。ニートな液体検体に空気を通してバブリングし、低温浴を用いて冷却することにより蒸気圧を制御した。固体二酸化炭素(ドライアイス)と3−ヘプタノンまたはエチレングリコールとの混合物により、それぞれ、−38℃および−15℃の浴温を与えた。氷水浴を用いて0℃の温度を与えた。蒸気圧便覧(Handbook of Vapor Pressure)(ヤウス・シー・エル(Yaws,C.L.),ガルフ・パブリッシング(Gulf Publishing):ヒューストン(Houston),1994年)のデータを用いてこれらの温度における各検体の蒸気圧を算出した。その後、多層フィルムの入ったセプタム密封バイアル中にステンレス鋼カニューレにより各空気/蒸気ストリームを流入させた。暴露時の各フィルムの色変化を視覚的にモニターし、複数回の観察により、平衡を確認した。表3は、濃度の関数として応答を示しており、「緑色」は、非暴露フィルムの色を示し、「桃色」は、飽和蒸気に対する応答を示し、「黄色」は中間の応答を示している。本発明の比色センサーフィルムを用いて蒸気の定性的な存在だけでなく検体の濃度をも決定できることが結果から示唆される。
センサーフィルム(実施例1のセンサーフィルム)を用いて水中の有機化合物の検出を行った。テトラヒドロフラン(THF)の水溶液(5体積%)内にフィルムを沈めたところ、緑色から黄色に目に見える色の変化が起こった。アセトンの水溶液(25体積%)中に沈めたところ、緑色から黄色〜緑色に目に見える色の変化が起こった。この実施例は、本発明の多層比色センサーフィルムにより水中の有機化合物の存在を検出できることを示している。純粋な水にフィルムを暴露したときには、色の変化は観察されなかった。
検出層をスピンコーティングすることにより、2つの多層センサーフィルムを作製した。ポリマー検出層を除けば、構造は同一であった。各センサーフィルムを作製するために、50μmポリエステル基材層上にバッチ式真空コーターで電子ビーム蒸発(蒸発速度2.5nm/秒)させることにより、アルミニウム反射層(100nm)を堆積させた。ポリ(スチレン)検出層およびポリ(メチルメタクリレート)検出層を、それぞれ、スピンコーティングにより1つのアルミニウムコーテッド基材上に堆積させた。それぞれ、5%(w/w)および9.4%(w/w)の濃度のトルエン溶液により、ポリマーをコーティングした。3500rpmで25秒間かけてスピンコーティングを行った。得られたポリマーの厚さは、260nm(ポリ(スチレン))および500nm(ポリ(メチルメタクリレート))であった。その後、実施例1のときに等しいスパッタリング条件により、クロム層(5nm)を各高分子表面上に堆積させ、多層センサーフィルム構成体を完成させた。センサーフィルムを飽和クロロホルム蒸気に暴露したところ、紫色から青色に(ポリ(スチレン))および桃色から薄緑色に(ポリ(メチルメタクリレート))可逆的なカラーシフトを起こした。フィルムをトルエン蒸気に暴露したところ、干渉に基づく色が永久的に消失した。このことは、フィルムから検体を除去したときにそのもとの色を回復できなかったことから示唆される。透過電子顕微鏡法(TEM)実験によると、この不可逆変化はアルミニウム層がスタックの残りの部分から離層したことが原因であることが示唆される。この実施例から、スピンコーティングにより多層比色センサーを作製できることが実証される。また、センサーの作製に使用される材料および方法を適切に選択することにより、本発明のセンサーの永久的な外観変化を実現できることが実証される。
実施例1に記載されているものと同一の全体構造および組成を有する2つの多層フィルムを作製した。ただし、サンプル6Aでは検出層の厚さは500nmであるのに対して、サンプル6Bでは厚さは650nmであった。フィルムは両方とも、実施例1のときと同様にラウリルアクリレート/IRR214/EB170混合物の重合により作製された検出層を含んでいた。一連の蒸気に対する2つのフィルムの応答を表4に示す。個々のセンサーはいずれもすべての検体を同定することはできないが(すなわち、6Aではトルエンとアセトンとが識別されず、6Bではアセトニトリルとアセトンとが識別されない)、両方のセンサーを組み合わせた応答は、試験したそれぞれの種に特有である。検体同定のために2つ以上の特有の多層フィルムを含むセンサーアレイの有用性が、この実施例により実証される。
Claims (3)
- 検体の存在および濃度の一方または両方を測定するための比色センサーであって、
実質的に連続な反射層と;
前記反射層上に存在する検出層であって、少なくとも1種のポリマー成分を含み、前記検体に暴露されたときに光学的厚さの変化が可能である検出層と;
前記検出層上に存在する実質的に連続な半反射層であって、金属または金属酸化物を含み、前記検出層の屈折率と異なる屈折率を有し、前記検体に対して浸透性である実質的に連続な半反射層と;
を含む、比色センサー。 - 検体の存在および濃度の一方または両方を測定するための比色センサーであって、
実質的に連続な反射層と;
前記反射層上に存在する検出層であって、異なるポリマー成分を含む2層以上のサブ層を含み、当該センサーが前記検体に暴露されたときに目に見えるパターンを形成するように前記異なるポリマー成分が前記2層以上のサブ層中に配置されている検出層と;
前記検出層上に存在する実質的に連続な半反射層であって、金属または金属酸化物を含み、前記検出層の屈折率と異なる屈折率を有し、前記検体に対して浸透性である実質的に連続な半反射層と;
を含む、比色センサー。 - 検体の存在または不在を検出する方法であって、
実質的に連続な反射層と;
前記反射層上に存在する検出層であって、少なくとも1種のポリマー成分を含み、前記検体に暴露されたときに光学的厚さの変化が可能である検出層と;
前記検出層上に存在する実質的に連続な半反射層であって、金属または金属酸化物を含み、前記検出層の屈折率と異なる屈折率を有し、前記検体に対して浸透性である実質的に連続な半反射層と;
を含む、比色センサーを提供することと、
光源を提供することと、
前記センサーを、検体が含まれる可能性のある媒体に接触させることと、
光学的性質の変化を前記センサーによりモニターすることと、
を含む、方法。
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- 2003-08-18 JP JP2004541478A patent/JP4391944B2/ja not_active Expired - Fee Related
- 2003-08-18 WO PCT/US2003/025711 patent/WO2004031760A1/en active Application Filing
- 2003-08-18 EP EP03799261A patent/EP1546701A1/en not_active Ceased
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2008
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KR20120018367A (ko) * | 2009-05-22 | 2012-03-02 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | 다층 비색 센서 |
KR101708076B1 (ko) | 2009-05-22 | 2017-02-17 | 쓰리엠 이노베이티브 프로퍼티즈 컴파니 | 다층 비색 센서 |
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CN100425987C (zh) | 2008-10-15 |
CN1685225A (zh) | 2005-10-19 |
EP1546701A1 (en) | 2005-06-29 |
WO2004031760A1 (en) | 2004-04-15 |
AU2003263862A1 (en) | 2004-04-23 |
US8506902B2 (en) | 2013-08-13 |
US20090035179A1 (en) | 2009-02-05 |
US20040062682A1 (en) | 2004-04-01 |
JP2006501467A (ja) | 2006-01-12 |
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