JP2005524857A - 活性表面増強ラマン分光(sers)基板としての金属被覆ナノ結晶性シリコン - Google Patents
活性表面増強ラマン分光(sers)基板としての金属被覆ナノ結晶性シリコン Download PDFInfo
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- JP2005524857A JP2005524857A JP2004513716A JP2004513716A JP2005524857A JP 2005524857 A JP2005524857 A JP 2005524857A JP 2004513716 A JP2004513716 A JP 2004513716A JP 2004513716 A JP2004513716 A JP 2004513716A JP 2005524857 A JP2005524857 A JP 2005524857A
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Abstract
Description
本明細書に使用する単数形の名詞は、一つまたは一つ以上の品目を意味する。
ナノ結晶性シリコン
本発明のある実施形態は少なくとも1層のナノ結晶性シリコンを有する装置300に関する。様々なナノ結晶性シリコン製造法が公知である(例えばペトロワ−コッホ(Petrova−Koch)ら、“迅速熱酸化多孔質シリコン−優れた燐光性Si(Rapid−thermal−oxidized porous silicon−the superior photoluminescent Si)”、アプライド フィジクス、レターズ(Appl.Phys.Lett.)、61:943、1992;エデルベルグ(Ederberg)ら、“プラズマ増強化学蒸着で製造されたナノ結晶性シリコンフィルムからの可視燐光(Visible luminescence from nanocrystalline silicon films produced by plasma enhanced vapor deposition”、アプライド フィジクス、レターズ(Appl.Phys.Lett.)、68:1415−1417、1996;シェーンフェルド(Schoenfield)ら、“ナノ結晶性シリコンにおけるSi量子ドットの作成(Foematon of Si quantum dots in nanocrystalline silicon)”、修飾された半導体構造に関する第7回国際会議プロシーディングス(Proc.7th Int.Conf.on Modulated Semiconductor Structures)、マドリッド(Madrid)、p605−608、1995;ザオ(Zao)ら、“ナノ結晶性Si:Si量子ドットで製造した材料(Nanocrystalline Si:a material constructed by Si quantum dots)”、低次元構造および装置に関する第1回会議(1st Con.on Low Dimensional Structure and Devices)、シンガポール(Singapore)、p467−471、1995;ルーツェン(Lutzen)ら、“非晶質シリコンのアニーリングで製造した超薄膜ナノ結晶性シリコンフィルムの構造的特徴(Structural characteristics of ultrathin mamocrystalline silicon films formed by annealing amorphous silicon)”、ジャーナル オフ バキューム サイエンス テクノロジー(J.Vac.Sci.Technology)、B16:282−05、1998;米国特許第5,770,022号;第5,994,164号;第6,268,041号;第6,294,442号;第6,300,193号)。本明細書に開示される方法と装置300はナノ結晶性シリコンの製造法に限られず、任意の方法も使用し得ると理解される。
本発明のある実施形態は、ラマン活性金属被覆基板240、340を使用する装置300および方法に関する。様々な実施形態で、基板はナノ結晶性多孔質シリコン110、210を含む。上記の議論の如く、基板110、210は純シリコンに限定されず、窒化シリコン、ゲルマニウムおよび/またはチップ製造業者に公知の他の物質も包含し得る。金属核化触媒および/またはドーパント等の他の微量物質も存在し得る。唯一の要請は、基板物質が図2に例示する様にラマン感受性金属で被覆し得る多孔質基板110、210を形成し得るものでなければならないことである。多孔質シリコンは783m2/cm3もの大きな表面積を有し、表面増強ラマン分光技術のための極めて大きい表面を提供する。
多孔質シリコン基板110、210を金、銀、白金、銅またはアルミニウム等のラマン活性金属で、公知の任意の方法で被覆し得る。この方法の非限定例には電気めっき、陰極電気移動、金属の蒸発とスパッタリング、メッキを触媒する種結晶の使用(即ち、金めっきのための銅/ニッケル種結晶の使用)、イオン注入、拡散、またはシリコン基板110、210、240、340上に金属薄膜をメッキするための任意の他の方法(例えばロペス(Lopez)およびフォーチェット(Fauchet)、“多孔質シリコン1次元フォトンバンドギャップ構造からのエルビウム放射(Erbium emission from porous silicon one dimensional photonic band gap structure)”、アプライド フィジクス レターズ(Appl.Phys.Lett.)、77:3740−6、2000;米国特許第5,561,304号;第6,171,945号;第6,359,276号参照)がある。金属被覆のその他の非限定例には無電解めっきがある(ゴール(Gole)ら、“直接電気接触のための無電解溶液から多孔質シリコンのパターン金属化(Patterned metallization of porous silicon from electroless solution for direct electrical contact)”、ジャーナル オフ エレクトロケミカル ソサイエティ(J.Electrochem.Soc.)、147:3785、2000)。金属層の組成および/または厚さを、金属被覆多孔質シリコン240、340のプラズモン共鳴周波数を最適化する様に制御する事が出来る。
本発明のある実施形態では、金または銀ナノ粒子等のラマン活性金属粒子を、ラマン信号をさらに増強するため金属被覆多孔質シリコン基板240、340に添加する事が出来る。本発明の様々な実施形態では、直径1nm〜2μmのナノ粒子を使用し得る。本発明のまた別な実施形態では、直径2nm〜1μm、5nm〜500nm、10nm〜200nm、20nm〜100nm、30nm〜80nm、40nm〜70nm、または50nm〜60nmのナノ粒子が検討される。本発明のある実施形態では、平均直径10〜50nm、50〜100nmまたは約100nmのナノ粒子が考慮される。ナノ粒子のサイズは金属被覆多孔質シリコン240、340中の細孔の直径に依存し、ナノ粒子が最高の内部にはまり込む様に選ばれる。ナノ粒子の形はほぼ球形であるが、任意の形または不規則な形のナノ粒子を使用してもよい。ナノ粒子の製造法は公知である(例えば米国特許第6,054,495号;第6,127,120号;第6,149,868号;リー(Lee)およびマイセル(Meisel)、ジャーナル オフ フィジカル ケミストリー(J.Phys.Chem.)、86:3391−3395、1982)。ナノ粒子はまた、ナノプリズムの形でも製造し得る(ジン(Jin)ら、“銀ナノスフェアのナノプリズムへの光誘発転換(Photoinduced conversion of silver nanospheres to nanoprism)”、サイエンス(Science)、294:1901、2001)。市販品からナノ粒子を入手する事も出来る(例えばナノプローブ社(Nanoprobes、Inc.、)、ヤファンク(Yaphank)、NY;ポリサイエンス社(Polyscience、INC.)、ワーリントン(Warrington、PA)。
本発明のある実施形態では、ラマン活性金属被覆多孔質シリコン基板230、340を大きな装置300および/またはシステムに組み込む事が出来る。ある実施形態では、基板230、340をマイクロ電気機械(MEMS)に組み込む事が出来る。MEMSは機械要素、センサー、アクチュエータおよび電子回路を備える複合システムである。これらの部品は全て、シリコン系または等価の基板でなる共通のチップ上に、公知のマイクロ加工技術により製造し得る(例えばボルドマン(Voldman)ら、アニューアル レビュー オフ バイオメディカル エンジニアリング(Ann.Rev.Biomed.Eng.)、1:401−425、1999)。MEMSのセンサー部品は機械的、熱的、生物学的、化学的、光学的および/または電磁現象を測定するために使用し得る。電子回路はセンサーからの情報を処理し、ポンプ、バルブ、ヒーター、クーラー、フィルター等のアクチュエータ部品を制御し、MEMSの機能を制御し得る。
ラマン検出器
本発明のある実施形態では、ラマン分光の任意の公知の方法で被分析試料を検出および/または同定する事が出来る。この様な実施形態において、ラマン活性基板240、340を少なことも1個のラマン検出ユニットと動作可能に結合させる事が出来る。ラマン分光による被分析試料の検出の様々な方法は公知である(例えば米国特許第6,002,471号;第6,040,191号;第6,149,868号;第6,173,677号;第6,313,914号参照)。表面増強ラマン分光(SERS)、表面増強共鳴ラマン分光(SERRS)、ハイパーラマン分光およびコヒーレント反ストークスラマン分光(CARS)の変法が開示されている。SERSおよびSERRSでは、ラマン検出の感度は銀、金、白金、銅またはアルミニウム表面等の粗い金属表面に吸着された分子で106倍以上に増加する。
本発明のある実施形態には、少なくとも1個の被分析試料に標識を付着させ、ラマン検出ユニット360による測定を助長する方法が含まれる。ラマン分光に使用し得る標識の非限定例にはTRIT(テトラメチルローダミンイソチオール)、NBD(7−ニトロベンズ−オキサ−1、3−ジアゾール)、テキサスレッド染料、フタル酸、テレフタル酸、イソフタル酸、クレジルファストバイオレット、クレジルブルーバイオレット、ブリリアンクレジルブルー、パラアミノ安息香酸、エリスロシン、ビオチン、ジオキシゲニン、5−カルボキシ−4’、5’−ジクロロ−2’、7’−ジメトキシフルオレッセイン、5−カルボキシ−2’、4’、5’、7’−テトラクロロフルオレッセイン、5−カルボキシフルオレッセイン、5−カルボキシローダミン、6−カルボキシローダミン、6−カルボキシメチルアミノフタロシアニン、アゾメチン、シアニン、キサンチン、スクシニルフルオレッセイン、アミノアクリジン、カンタムドット、カーボンナノチューブおよびフレーレンが含まれる。これらの、またはそれ以外のラマン標識は市販されている(例えばモレキュラープローブ社(Molecular Probe Inc.、オイゲン(Eugen)、OR);シグマアルドリッチケミカル社(Sigma Aldrich Chemical Co.、セントルイス(St.Louice)、MO)および/または公知の方法で合成できる。
本発明のある実施形態では、装置100、300はコンピュータ160、395を包含し得る。実施形態はコンピュータ160、395のタイプに限定されない。コンピュータ160、395の例には情報を伝達するバス、および情報を処理する演算装置が含まれる。ある実施形態では、演算装置はインテル社(Intel Corp.、サンタクララ(Santa Clara)、CA)が市販するペンティアム(Pentium(登録商標))IIファミリー、ペンティアムIIIファミリーおよびペンティアムIVファミリーを含むペンティアムファミリーの演算装置から選ばれるが、それに限定されない。本発明の別な実施形態では、演算装置はセレロン(Celeron(登録商標))、イタニウム(Itanium(登録商標))、ペンティアムジオン(Pentium Xeon(登録商標))演算装置(インテル社(Intel Corp.)、サンタクララ(Santa Clara)、CA)である。本発明の様々な他の実施形態では、演算装置はインテルIA−32またはインテルIA−64等のインテル基本設計に基づくものである。または、他の演算装置も使用し得る。
多孔質ナノ結晶性シリコンの作成
多孔質シリコン110、210を公知の技術(ロペス(Lopez)およびフォーチェット(Fauchet)、2000)を用いて陰極電気移動により金属被覆する事が出来る。本実施例の目的では金属被覆に銀が使用されるが、金または白金等の他の金属も使用し得る。多孔質シリコン表面110、210を洗浄し、ロペスおよびフォーチェットの方法に従って電気移動で銀を被覆する(アプライド フィジクス レターズ(Appl.Phys.Lett.)、75:3989、1999)。当業者は、公知の任意の多孔質シリコン基板110、210上に薄膜を生成する技術を、本発明の様々な実施形態で使用し得ることを理解できると思われる。
上記に開示された様に作成したラマン活性金属被覆基板240、340を、図3に示す被分析試料のラマン検出、同定および/または定量用の装置300中に組み込む。基板240、340を例えば入り口320および出口350チャネルに接続されたフロースルーセル330に組み込む。入り口チャネル320を、試料インジェクター310および/または反応チャンバー310等の少なくとも1台の他の装置310に接続する。被分析試料はフローセル330に入りラマン活性基板340を横切って流れ、ラマン検出ユニット360で検出される。検出ユニット360はラマン検出器380とレーザー370等の光源370を備える。レーザー370は励起光線390を放射し、被分析試料を活性化しラマン信号を放射する。ラマン信号は検出器380で検出される。本発明のある実施形態では、検出器380はコンピュータ395と接続されて作動し、試料中に存在する被分析試料に関するデータを処理、解析、記憶および/または転送する。
Claims (30)
- a)金属被覆多孔質基板を作成する段階と、
b)前記基板を少なくとも1個の被分析試料試を含む試料にさらす段階と、
c)少なくとも1個の被分析試料を検出および/または同定のためにレーザー励起および分光を用いる段階と
を備える、方法。 - 前記基板が多孔質半導体基板である、請求項1に記載の方法。
- 前記基板がナノ結晶性シリコン、単結晶シリコン、多結晶シリコン、非晶質シリコンおよびレーザーでアニールされたシリコンからなる群から選択される、請求項2に記載の方法。
- 金属ナノ粒子が前記金属被覆多孔質基板に添加される、請求項1に記載の方法。
- 前記金属被覆が銀、金、白金、銅および/またはアルミニウムを含む、請求項1に記載の方法。
- 前記分光がラマン分光である、請求項1に記載の方法。
- 前記ラマン分光が表面増強ラマン分光(SRRS)、表面増強共鳴ラマン分光(SERRS)、ハイパーラマンおよび/または反ストークスラマン分光(CARS)である、請求項6に記載の方法。
- 前記被分析試料がアミノ酸、ペプチド、ポリペプチド、タンパク質、糖タンパク質、リポタンパク質、ヌクレオシド、ヌクレオシド、オリゴヌクレオチド、核酸、糖、炭水化物、オリゴ糖、多糖、脂肪酸、脂質、ホルモン、代謝物、サイトカイン、ケモカイン、受容体、神経伝達物質、抗原、抗体、基質、代謝物、コファクター、阻害剤、薬剤、医薬品、栄養物、プリオン、毒素、毒、爆発性物質、殺虫剤、化学兵器、生物兵器、バクテリア、ウイルス、放射性同位元素、ビタミン、複素環式芳香族化合物、発癌性物質、突然変異原、麻酔剤、アンフェタミン、バルビツール酸塩、幻覚発現物質、廃棄物および/または汚染物を含む群から選ばれる、請求項1に記載の方法。
- 前記被分析試料がヌクレオシド、ヌクレオチド、オリゴヌクレオチド、核酸、アミノ酸、ペプチド、ポリペプチドまたはタンパク質である、請求項8に記載の方法。
- 前記少なくとも1個の被分析試料が少なくとも1個のラマン標識でラベルされている、請求項1に記載の方法。
- 各被分析試料が識別可能なラマン標識でラベルされている、請求項10に記載の方法。
- 少なくとも1個の捕捉分子が金属被覆多孔質シリコン基板に付着している、請求項1に記載の方法。
- 前記捕捉分子がオリゴヌクレオチド、核酸、抗体、抗体断片、抗原、エピトープ、レシチン、タンパク質、ポリペプチド、ペプチド、受容体タンパク質、リガンド、ホルモン、ビタミン、代謝物、基質、阻害剤、コファクター、医薬品、アプタマー、サイトカインおよび神経伝達物質を含む群から選ばれる、請求項12に記載の方法。
- a)金属被覆ナノ結晶性多孔質シリコン基板と、
b)レーザーと
c)ラマン検出器と
を備える、装置。 - 前記多孔質シリコンを犠牲層として使用する、請求項14に記載の装置。
- 前記犠牲層が金属で置き換えられる、請求項15に記載の装置。
- 金属ナノ粒子を更に有する、請求項14に記載の装置。
- 前記金属が銀、金、白金、銅および/またはアルミニウムを有する、請求項14に記載の装置。
- 前記ラマン検出器と動作可能に結合するコンピュータを更に備える、請求項14に記載の装置。
- ラマン検出器と動作可能に結合するフロースルーセルを更に備え、前記フロースルーセル内部の前記金属被覆ナノ結晶性多孔質シリコン基板を通って流体が流れる、請求項14に記載の装置。
- 前記金属被覆多孔質シリコン基板がマイクロ電気機械システム(MEMS)中に組み込まれる、請求項14に記載の装置。
- 前記金属被覆多孔質シリコン基板が集積チップの一部として構成される、請求項21に記載の装置。
- 前記金属被覆多孔質シリコン基板がウェーハから取り出され、MEMSに組み込まれる、請求項21に記載の装置。
- 金属被覆ナノ結晶性多孔質シリコンの層を備えるウェーハ。
- 前記金属被覆が銀、金、白金、銅および/またはアルミニウムを含む、請求項24に記載のウェーハ。
- 前記多孔質シリコンがシリコン、酸化シリコン、二酸化シリコンおよび/または窒化シリコンを含む、請求項24に記載のウェーハ。
- 前記多孔質シリコンが金属で被覆される前に二酸化シリコンによって酸化される、請求項24に記載のウェーハ。
- a)表面積の大きい金属被覆材料を調製する段階と、
b)材料を少なくとも1個の被分析試料を含む試料にさらす段階と、
c)レーザー励起と分光を用いて少なくとも1個の被分析試料を検出および/または同定する段階と
を備える、方法。 - 前記表面積の大きい材料が多孔質シリコンである、請求項28に記載の方法。
- 前記分光がラマン分光である、請求項28に記載の方法。
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- 2003-05-16 WO PCT/US2003/015277 patent/WO2003106943A1/en active IP Right Grant
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- 2003-05-16 AU AU2003232139A patent/AU2003232139A1/en not_active Abandoned
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- 2003-06-11 TW TW092115837A patent/TWI290621B/zh not_active IP Right Cessation
- 2003-06-12 MY MYPI20032186A patent/MY134271A/en unknown
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JP2005283556A (ja) * | 2004-03-05 | 2005-10-13 | Canon Inc | 標的物質認識素子、検出方法及び装置 |
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JP4579593B2 (ja) * | 2004-03-05 | 2010-11-10 | キヤノン株式会社 | 標的物質認識素子、検出方法及び装置 |
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JP2006284335A (ja) * | 2005-03-31 | 2006-10-19 | Univ Nagoya | クロロフィル蛍光測定方法およびクロロフィル蛍光測定装置 |
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JP2013151758A (ja) * | 2008-03-07 | 2013-08-08 | Japan Science & Technology Agency | 複合材料 |
JP2012508881A (ja) * | 2008-11-17 | 2012-04-12 | ヒューレット−パッカード デベロップメント カンパニー エル.ピー. | 表面増強ラマン散乱(sers)用基板 |
US8547549B2 (en) | 2008-11-17 | 2013-10-01 | Hewlett-Packard Development Company, L.P. | Substrate for surface enhanced Raman scattering (SERS) |
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JP2016539335A (ja) * | 2013-11-28 | 2016-12-15 | ライカ マイクロシステムズ シーエムエス ゲゼルシャフト ミット ベシュレンクテル ハフツングLeica Microsystems CMS GmbH | Cars顕微鏡法による試料の検査方法 |
Also Published As
Publication number | Publication date |
---|---|
TWI290621B (en) | 2007-12-01 |
US6970239B2 (en) | 2005-11-29 |
WO2003106943A1 (en) | 2003-12-24 |
EP1511980A1 (en) | 2005-03-09 |
HK1071427A1 (en) | 2005-07-15 |
CN1659425A (zh) | 2005-08-24 |
ATE372505T1 (de) | 2007-09-15 |
CN1659425B (zh) | 2011-01-26 |
DE60316150D1 (de) | 2007-10-18 |
KR100990580B1 (ko) | 2010-10-29 |
TW200407536A (en) | 2004-05-16 |
MY134271A (en) | 2007-11-30 |
JP4347801B2 (ja) | 2009-10-21 |
EP1511980B1 (en) | 2007-09-05 |
US20030231304A1 (en) | 2003-12-18 |
AU2003232139A1 (en) | 2003-12-31 |
DE60316150T2 (de) | 2008-06-05 |
KR20050013571A (ko) | 2005-02-04 |
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