JP5335371B2 - 新規材料の組合せ合成方法 - Google Patents
新規材料の組合せ合成方法 Download PDFInfo
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- JP5335371B2 JP5335371B2 JP2008278792A JP2008278792A JP5335371B2 JP 5335371 B2 JP5335371 B2 JP 5335371B2 JP 2008278792 A JP2008278792 A JP 2008278792A JP 2008278792 A JP2008278792 A JP 2008278792A JP 5335371 B2 JP5335371 B2 JP 5335371B2
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- substrate
- reaction
- monomer
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
- Y10T428/31931—Polyene monomer-containing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
- Y10T436/2525—Stabilizing or preserving
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
- Y10T436/25375—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.]
- Y10T436/255—Liberation or purification of sample or separation of material from a sample [e.g., filtering, centrifuging, etc.] including use of a solid sorbent, semipermeable membrane, or liquid extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T436/00—Chemistry: analytical and immunological testing
- Y10T436/25—Chemistry: analytical and immunological testing including sample preparation
- Y10T436/25875—Gaseous sample or with change of physical state
Description
前記の方法を用いて新しい一群のジャイアント磁気抵抗性(GMR)コバルト酸化物を発見した。薄膜蒸着技術をマスキング技術と併用すると、Ln1-xMxCoOz(式中、Lnは、例えばY及びLaであり、Mは、例えばPb、Ca、Sr及びBaであり、xは約0.1から約0.9の範囲の値を有し、そしてzは約2から約4の範囲の値を有する)の組成と化学量論関係を有する一群の材料アレイが形成された。一旦形成されたら、これら材料アレイをそれらの内で有用な性質を有する材料についてスクリーニングにかけた。更に詳しくは、これら材料アレイを、なかんずくジャイアント磁気抵抗性(GMR)を有する特定の材料についてスクリーニングにかけた。このようにスクリーニングを行うときに、大きな磁気抵抗性(MR)はLa1-x-(Ba,Sr,Ca)x-CoOz試料(式中、xは約0.1から約0.9の範囲の値を有し、そしてzは約2から約4の範囲の値を有する)に見いだされた。有用な性質を有する材料が同定されたら、そのような材料が更なる量で製造された。
I.用語
II.概略
III.基質上の反応部位の分離
IV.反応物成分の供給方法
A.薄膜付着法を用いる供給
B.ディスペンサーを用いる供給
V.多ターゲット薄膜付着システム
VI.支持体に対するディスペンサーの移動
VII.成分アレイ(array)を反応させるための合成経路
VIII.物質アレイをスクリーニングする方法
IX.代替の態様
X.実施例
A.16酸化銅薄膜物質のアレイの合成
B.128酸化銅薄膜フィルム物質のアレイの合成
C.BiSrCaCuOとYBaCuOを含む128個の酸化銅薄層材料のアレイの合成
D.酸化コバルトの薄層材料アレイの合成
E.16の異なる有機高分子のアレイの合成
F.ゼオライトアレイの合成
G.噴霧沈積法を用いた酸化銅化合物のアレイの合成
H.16個の異なった亜鉛珪酸塩リン光体のアレイの合成
I.スパッター法とフォトリソグラフィー遮蔽法の組み合わせを用いた酸化銅の薄いフイルム材料のアレイの合成
XI.結論
ここで使用される以下の用語は以下の意味を有する。
(a)金属間化合物(または中間構成要素):金属間化合物は、臨界点温度以下で長距離秩序の結晶構造を形成する金属材料特有のものである。このような材料は、特定の割合で結合した2つの金属の原子が、その2つの金属の構造とは異なる構造の結晶を形成する(例えば、NiAl,CrBe2,CuZnなど)。
(b)金属合金:金属の特性をもち、少なくとも1つが金属である2つ以上の化学物質を混合した組成物。
(c)磁性合金:シリコン−鉄などの強磁性を示す合金や、少量の他の元素(例えば、銅、アルミニウム、クロム、モリブデン、バナジウムなど)を含んだ鉄−ニッケル合金、あるいは鉄−コバルト合金などである。
(d)セラミックス:通常、セラミックスとは、酸化金属やホウ酸化物、炭化物、窒化物あるいはこれらの材料を混合したものを指す。セラミックスは、無機物、非金属、非分子固体であり、単結晶材料及び結晶構造材料の双方を有する。ここでは、本発明を用いた特性で形成、スクリーニングされる材料の実例としてセラミックスが挙げられている。そのような材料は例えば、アルミナ、ジルコニウム、シリコン炭化物、窒化アルミニウム、窒化シリコン、YBa2Cu3O7-8超伝導体、La2-xSrxCuO4超伝導体、Bi2CaSr2Cu2O8+x超伝導体、Ba1-xKxBiO3超伝導体、ReBaCu超伝導体、フェライト(BaFe12O19)、ゼオライトA(Na12[(SiO2)12(AlO2)]・27H2O)、軟磁石、永久磁石、高比誘電率材料(BaTiO3)、ピエゾ材料(例えば、ジルコン鉛酸チタン酸塩(PZT)、NaNbO3,NaTaO3)、光電子材料(例えば、リチウムニオブ酸塩(LiNbO3))、ジャイアント磁気抵抗材料(GMR)などである。ここで用いられるジャイアント磁気抵抗材料は、磁界中での抵抗値が、無印加時より5%以上変化するのもの、つまり、抵抗値変化率の絶対値が5%以上のものをいう。
即ち、|ΔR/R|>5%であり、ここで、抵抗値の変化は次式で求められる。
ΔR/R=((磁界印加時の抵抗値)−(無印加時の抵抗値))/(無印加時の抵抗値)
(a)非生物有機ポリマー:多数の繰り返し単位による巨大分子から構成される非金属材料である。このような材料は、天然物として存在するだけでなく合成によっても生成可能であり、また架橋構造を有する場合もある。さらに、重合状態も多様であり、ホモポリマー、コポリマー、あるいはより高次のポリマー(例えば、ターポリマーなど)にもなりうる。「非生物」なので、α−アミノ酸やヌクレオチドなどは含まれない。さらに、「非生物有機ポリマー」としては、ビルディングブロックの線形あるいは段階的結合により合成されるポリマーは含まない。本発明の方法を用いて生成されるポリマーは、例えば、ポリウレタン、ポリエステル、ポリカーボネイト、ポリエチレンイミン、ポリアセテート、ポリスチレン、ポリアミド、ポリアニリン、ポリアセチレン、ポリピロールなどであるが、これらに限定されるものではない。
本発明は、既定領域に材料アレイを有する基材を生成及び使用するための方法及び装置を提供する。ここに記載される発明は、主に無機材料の生成に関するが、本発明を他の材料の生成にも適用することができる。本発明に含まれる方法で生成可能な材料は、例えば、共有結合型網状構造固体、イオン固体、分子固体などである。より詳細には、本発明に含まれる方法で生成可能な材料は、無機材料、金属間材料、金属合金、セラミック材料、有機材料、有機金属材料、非生物有機ポリマー、複合材料(例えば、無機物化合物、有機物化合物、またはこれらの組み合わせ)が含まれるが、これに限定されるものではなく、本発明の開示に基づいて当業者であれば生成可能な他の材料も含まれる。
好適な態様では、本発明の方法は単一の基質表面上の既知の位置における異なる物質のアレイを準備するのに用いられる。本質的に、発明において考えられるあらゆる基質が用いることができる。基質は有機、無機、生物学的、非生物学的、あるいはこれらの結合であって、粒子、糸状、沈殿、ゲル、シート、チューブ、球体、コンテナ、キャピラリー、パッド、スライス、フィルム、プレート、スライドなどとして存在しうる。基質は、例えば円板、球体、円などのいかなる便利な形を有していてもよい。基質は好適には平らで、しかし選択的に様々な表面形状をとってもよい。例えば、基質は異なる物質の合成が起こる膨らんだ、あるいはくぼんだ部位を含んでいてもよい。基質及び表面は好適には説明された反応が実行されるところに堅い支柱(support)を形成する。基質は、例えばポリマー、プラスチック、パイレックス(登録商標)、クオーツ、レジン、シリコン、シリカ又はシリカベースの物質、炭素、金属、無機ガラス、無機結晶、膜などを含む幅広く多様な物質であってもよい。他の基質物質は本開示のレビューにおいて当業者には容易に明らかになるであろう。固体基質表面は基質として同一の物質からなるが、あるいは選択的に異なることもありうる。すなわち基質が異なる物質で被覆されることもありうる。さらに、基質表面は関係ある成分が分配されるところに(例えばセルロースなどの)吸収材を含むことができる。最も好適には基質及び基質表面物質は合成される物質の種類に依存し、いかなる場合における選択も当業者には容易に明らかになるであろう。
本発明の供給システムにおいて、少量の正確に計量された量の各反応物成分を各反応領域に供給する。これは、種々の供給法単独かまたは種々の供給法と種々の物理的マスキング法もしくは写真平版法との組合わせを用いて行うことができる。本発明の方法に用いるのに適する供給法は、概して薄膜付着技術の使用を含む方法およびディスペンサーの使用を含む方法に分類することができる。
基質上の予め定めた領域に種々の反応物の薄膜を付着させるために物理的マスキング法または写真平版法と組合わせた薄膜付着法を用いることができる。このような薄膜付着法は一般に次の4つの部類に分けることができる:蒸発法、グロー放電法、気相化学的方法および液相化学的方法。これらの部類に含まれるものに、たとえばスパッター法、スプレー法、レーザーアブレーション法、電子ビームまたは熱蒸発法、イオン注入またはドーピング法、化学蒸着法のみならず集積回路の加工に用いられる他の方法がある。これらの方法はすべて、基質上の選ばれた領域に種々の反応物の極めて均一な層、すなわち薄膜を付着させるのに適用することができる。さらに、マスク、供給源および/または基質の相対的形状を調整することによって、このような薄膜付着法を、基質上の個々の反応領域、あるいはまた基質上のすべての反応領域に均一な勾配をつけるのに用いることができる。本発明の方法に用いることができる種々の薄膜付着法を概観するには、たとえばHandbook of Thin-Film Deposition Process and Techniques,NoyesPublication(1988)を参照されたい。同書はあらゆる目的のために本明細書に参考資料として集録してある。
前記の供給法に加えて、単一基質に小滴または粉末状の反応物成分の異種の組合せをつくるのにディスペンサーを用いることができる。さきに述べたように、毛細管から5ナノリットル以下の小滴容量を分取するのに市販のミクロピペット装置を用いることができる。このような小滴は非湿潤性マスクを用いる場合には直径300μm以下の反応領域に適合させることができる。若干の態様では、反応物溶液を付着させる前に後述のようにミクロピペットを反応領域の上に正確かつ精密に位置決めする。
帯電した液滴は、帯電円筒を通過後、電界ポテンシャル源234に接続されるそれぞれ230および232の2枚のプレート間にできる電界に入る。電界と各液滴の電荷との作用の結果として、液滴が有する電荷によってプレート間の中心線経路から液滴は偏向する。したがって、液滴が、任意に動いている記録媒体236上に落ちると、情報を信号として表わす付着パターンが記録媒体上に生じる。
さきに述べた薄膜付着法を行うのに用いた反応システムは、広範囲に異なることができ、かつ大半は薄膜付着技術が用いられているシステムによる。本発明は、本発明の方法を実施する上で用いることができる多数の種々の多ターゲット薄膜付着システムを提供する。本明細書に開示されるシステムの多くの態様や変形はこの開示を検討すれば当業者には明らかになろう。
本発明の方法に用いることができる8個のRFマグネトロンスパッタリングガンシステムの例を図10に示す。このシステムは8個のRFマグネトロンスパッタリングガン110を含み、各ガンは問題の反応物成分を含有している。8個のRFマグネトロンスパッタリングガンはディスク112の約2ないし5インチ上方に配設され、該ディスク112はその上に8個のマスキングパターン114のみならず8個のフィルム厚さモニター116を載せている。このシステムでは8個のRFマグネトロンスパッタリングガンのみならずディスクも固定されている。しかし、基質118は基質マニピュレータ120と結合され、該基質マニピュレータ120は直線および回転運動を行うことができ、かつ、スパッタリングが始まるときに基質をマスクと接触させるように基質を問題の特定マスクと係合させている。それぞれのマスクを通して各成分を逐次付着させることによって8成分の組合せが基質上に生成する。このシステム全体の真空中で用いられる。
組合せスパッタリングシステムの別の設計を図11に示す。このシステムは8個のRFメガトロンスパッタリングガン110を含み、各ガンは、完全な円形の反応チャンバー側面から挿入される問題の反応物成分を含有する。基質は直線および回転運動をするシャフト130に付着している。付着の間に基質自体は8個のRFマグネトロンスパッタリングガン110の任意の1つに面するように移動および回転することができる。基質は基質ホルダー132内に置かれ、基質ホルダーは基質を保持する以外に、基質118の上に1個の2次マスキングパターン134をしっかりと固着させる(1次マスクは基質上の反応部位の形と密度を限定して、全実施中固定されるグリッドである)。反応物成分の付着後、マニピュレータ138を用いて2次マスクを取り外し、それをカセット140内に入れ、次に必要な2次マスクを取り出して、このマスクを基質ホルダー132の上に置く。基質ホルダーの固定機構はマスクの整合を好ましくは25μm以内に保証する。(基質とマスクと25μmよりもよい精度で整合させる固定機構については多くの考案や設計があることは当業者には容易に明らかであろう。)図11に示す構造において、マニピュレータ138は垂直方向に直線運動をし、カセット140は水平方向に直線運動をする。このフォーマットにおいて、マニピュレータ138はカセット140内の任意の2次マスクを移動させるのに用いることができる。この設計は、好ましくは2個のマスクの使用、より好ましくは8個のマスクの使用、さらにより好ましくは20個のマスクの使用、なおさらにより好ましくは20個以上のマスクの使用にあてはまる。このシステムを用いると、問題の反応物成分のすべてを異なるマスキングパターンを通して付着させ、それによって積層薄膜前駆物質の組合せライブラリーをつくることができる。
前記の1つに関連する1つのシステムはカセット交換機構を有するパルスレーザー付着システムである。この設計は図12に示す。反応物成分はカルーセルホィール内に置き、該ホィールは少なくとも4個の反応物成分、より好ましくは少なくとも8個の反応物成分を保持することができる。別の方法は多角形142(図12参照)の異なる面に各反応物成分を置くことである。たとえば、多角形が十角形であれば、10個の反応物成分をそれに載せることができる。いずれの設計にせよ、目的は、特定時間の間に反応物成分をレーザービーム144の前に迅速に動かし、次にほとんど瞬間的に反応物成分を取換えることができることにある。カルーセル態様では、反応物成分は急速に回転してレーザービーム144と交わることができる。多角形態様では、レーザービーム144を固定する前面に所望の多角形の面を回転することによって反応物成分を交換することができる。
1,000個以上の物質を含むライブラリーを三成分、四成分及び五成分物質だけを含むように構築する場合、例えば含まれる種々の遮蔽工程の数はたやすく30に達する。さらに、各ライブラリーは幾つかの独自の遮蔽パターンを使用する必要があるらしい。そこで、それぞれ数秒以内で支持体の前に数百の異なる遮蔽パターンのうちの一つを作り出すことができるシステムを持つならば有利と言える。そのようなシステムを図13に例示する。
ディスペンサーを用いて正確に特定された領域に一貫して反応体飛沫をめっきさせるには、放出器械及び支持体に共通の基準枠が必要である。言い換えれば、その器械の基準座標を支持体の基準座標上に正確に位置づけなければならない。典型的には、反応領域のアレイを完全に位置づけるには支持体上のただ2点の基準点が必要なだけである。ディスペンサー器械はこれらの基準点の位置を突きとめた後にその内部基準座標を調整して必要な配位をとらせる。この後、ディスペンサーを特定の方向に特定の距離だけ移動させて既知の領域の上に直接位置させることができる。もちろん、このディスペンサー器械は正確に反復可能な移動を行わなければならない。さらに、アレイの個々の領域は基準マークが形成された後には支持体上の基準マークに対して位置を変えてはならない。あいにく、支持体の組み立て及び使用の間に一般に受ける圧力又は他の機械的作用がこの支持体を曲がらせて基準マークと反応領域の間の一致を変化させてしまうこともある。
成分アレイが支持体上の予め規定された領域に放出されると、幾つかの異なる合成経路を用いて成分を同時に反応させることができる。成分を、例えば合成技術、光化学技術、重合技術、鋳型特定合成技術、エピタキシャル成長技術に基づく溶液を用いて;又はゾル・ゲル処理;熱、赤外線若しくは電磁波加熱;焼成、焼結若しくは焼鈍;熱水作用法;融剤法;溶媒気化による結晶化等によって反応させることができる。他の有用な合成方法は当業者には本開示を見れば明らかとなろう。さらに、最も適当な合成経路は合成すべき物質の分類に依存し、与えられたケースにおける選択は当業者には容易に明らかとなるであろう。また、必要に応じて反応体成分を反応に先立って例えば超音波法、機械的方法等を用いて混合してもよいことは当業者には容易に明らかとなるであろう。このような技法は支持体上の所定の予め規定された領域に直接用いてもよく、或いは、支持体上の予め規定された領域全てに同時に用いてもよい(例えば、成分が有効に混合されるような方法で支持体を機械的に移動させてもよい)。
製造すると、有用な性質を持つ物質に対して物質アレイをスクリーニングすることができる。アレイ全体、或いはその一部(例えば、予め規定された領域の横列)のいずれかを平行に有用な性質を持つ物質に対してスクリーニングすることができる。物質アレイをスクリーニングするためにスキャニング検出システムを好ましくは利用するが、単位面積当たりの領域密度は.04領域/cm2よりも大きく、より好ましくは0.1領域/cm2よりも大きく、さらにより好ましくは1領域/cm2よりも大きく、さらにより好ましくは10領域/cm2よりも大きく、なおいっそう好ましくは100領域/cm2よりも大きくなる。最も好ましい態様においては、物質アレイをスクリーニングするためにスキャニング検出システムを好ましくは利用するが、単位面積当たりの領域密度は1,000領域/cm2よりも大きく、より好ましくは10,000領域/cm2よりも大きく、さらにより好ましくは100,000領域/cm2よりも大きく、なおいっそう好ましくは10,000,000領域/cm2よりも大きくなる。
本発明の他の態様において、少なくとも2種の、異なったアレイの物質群が、実質的に同じ濃度の実質的に同じ反応成分を、第1及び第2基体の両方の上の前以て定義された領域に送り、その後、広いアレイの組成で、第1基体上の成分を1組みの第1反応条件にかけ、そして第2の基体上の成分を1組みの第2反応条件にかけることによって製造される。もし、例えば第1基体が該基体上の第1領域上に成分A及びB、さらに該基体上の第2領域上に成分X及びYを有すると、第2基体はその上の前以て決定された領域内に実質的に同じ成分を有するように製造される。すなわち、第2基体は、その上に含まれる成分において第1基体と実質的に同じである。そういうものとして本例において、第2基体も該基体上の第1領域上に成分A及びB、さらに該基体上の第2領域上に成分X及びYを有する。
(a)単一の基体上に、一定アレイの異なる物質群を形成すること;(b)有用な性質を有する物質のためのアレイをスクリーニングすること;並びに(c)追加量の、有用な性質を有する物質をつくることを含む方法によって製造される。このような物質は、例えば金属間物質、金属アロイ、セラミック物質、有機金属物質、有機ポリマー、複合材料(例えば無機複合材料、有機複合材料またはこれらの組み合わせ)等を含む。さらに、有用な性質は例えば電気的、熱的、機械的、形態学的、光学的、磁気的、化学的なもの等を含む。
下記の実施例は本明細書において本発明の効果を説明するために提供される。
この実施例は酸化銅薄膜物質のアレイの合成及びスクリーニングを明らかにする。そのリアクタント(reactant)は、(100)光沢化された表面を持った1.25cm×1.25cmMgOに伝達(deliver)された。その上の16の予め定められた地域を持つ基板は、真空中において反応室内に含まれた。そのリアクタントは、2元のマスキング技術と組合せたスパッタリング(sputtering)システムを使用して薄膜の形でその基板に伝達された。その二元マスクはステンレス鋼から作られた。RF磁電管ガン(gun)スパッタリングシステムはその基板上に予め定められた地域にリアクタント成分を伝達するために使用された。使用されたそのRF磁電管スパッタリングガン(US,インク,Campbell,CA)によって製造されたMini・マック(mak)は直径約1.3インチであった。50〜約200WのRFインプットパワー(マッチングネットワーク(matchingnetwork)でのPlasmthern−2000によって供給された)では、析出(deposit)速度は5つの異なったリアクタント成分のために約0.3Å/s〜約2Å/sの範囲であった。そのRFスプレーヤ(sprayer)は基板の上方約3〜4インチのところに位置し、そして析出されたフィルムの均一性は1〜2インチ直径区域上約5%であった。そのスパッタリングガス流れ(Ar又はArとO2)は計量バルブ及び手動ゲートバルブを通して異ったポンプ輸送によって管理された。高い析出速度を達成するために最良のガス圧範囲は、約5〜15mTorrであった。そのチャンバーにおける各ガス成分の部分圧は残留ガス分析器(Ferran Scientitic,カリフォルニア州サンジエゴによるMicropole Sensor)を使用し異なるポンプ輸送なしに15mTorrまで直接モニターされた。
この実施例は異った組合せ、化学量論及びBi,Ca,Cu,Pb及びSrの析出シークエンス(sequence)からなる128メンバーライブラリの合成及びスクリーニングを説明する。そのライブラリは、RF磁電管スパッタリングガンを使用して物理的マスクを通してターゲット(tarhet)物質をスパッタリングして発生された。スパッタリングは、スパッタリングガスとして空気で10-3〜10-6Torrで実施され、析出速度は0.1〜1Å/秒であった。フィルム析出厚さは、結晶ミクロバランスでモニターされ、そしてプロフィロメーターで独立に調整された。その析出されたフィルムの均一性は2−インチ直径区域にわたって約5%変化した。(100)光沢化された表面を持ったMgO単一結晶は基体として使用され、そしてCuO,Bi2O3,CaO,PbO及びSrCO3はスパッタリングターゲットとして使用された。そのライブラリは128(1×2mm)の穴を含む第一元物理的マスクを一連の第二元マスク(図21)に重ね合わせることにより二元マスキングストラーテッジ(strategy)を使って発生された(Fodor,S.P.A.etal.,Science251,767(1991)参照)。前駆物質は一歩ずつ(stepwise)のやり方で適当な二元マスクを通してスパッタ(sputter)された。6つの同等の128メンバーまで、ライブラリは同時に合成できそして異った条件で処理できた。二元合成において、2m化合物は与えられた数のステップ(m)のマスキングのために形成された。そのアレイは、全体の析出/マスキングシークエンスから1つ又はそれ以上の工程を削除することによって形成できるすべての組合せを含む。追加のマスキングスキーム(scheme)は、他のライブラリ、例えば10個の前駆体から誘導されたすべての第四級化合物からなるライブラリを発生させるために使用されることができる。
本実施例は、Ba,T,Bi,Ca,Sr,Cuの異なる組み合わせ、当量関係、蒸着手順からなる128のライブラリの合成とスクリーニングを説明する。RFマグネトロンスパッタリング銃を用いて蒸着材料を物理的にマスクしてスパッタリングすることにより生成される。スパッタリングは10-5から10-6Torrの真空下で、アルゴンをスパッタリングガスとして行われる;蒸着速度は0.1から1s-1であった。薄層の厚みは結晶ミクロ天秤(STM-100,サイコン・インスツルメンツ社ニューヨーク州シラキュース、米国)で測定し、プロファイロメーターで独立に較正した。蒸着した薄層の均一度は、1インチから2インチ経の範囲で約5%であった。酸化マグネシウムの研磨した011面を基質として用い、BaCO3,Y2O3,Bi2O3,CaO,SrCO3,CuOをスパッタリング物として用いた。ライブラリは下記に示す非バイナリマスク法によって生成した。
本実施例は、酸化コバルト薄層材料アレイの合成とスクリーニングを説明する。2.5cmx2.5cmのLaAlO3基板の研磨した100面へ反応物を添加した。128の予め画定された領域をその上に有する基板を真空中で反応器へ入れた。反応物は非二進法マスキング法との組み合わせたスパッタリング法により基板上へ薄層として形成された。使用されたマスクはステンレス製である。反応物の組成体を基板上の予め画定された領域へ送出するのにはRFマグネトロンスパッタリング銃を用いた。RFマグネトロンスパッタリング銃(Mini-mak、USインコーポレーション社製、キャンベル、カリフォルニア州、米国)は約1.3インチの内径を有する。RF入力(Plasmtherm-2000から同期ネットワークにより供給される)50から200Wで、蒸着速度は種々の反応組成物に応じて0.3/sから約0.2/sの範囲であった。RFマグネトロン噴霧器は基板から3から4インチ上に設置され、蒸着フィルムの均一度は、1インチから2インチ径の範囲で約5%であった。スパッタリングガス流量(アルゴンまたはアルゴンと酸素)は計量バルブと示差式ポンプにより手動ゲートバルブを通して制御した。速い蒸着速度を実現するために最も好ましい圧力は5から15mTorrであった。反応器内のそれぞれの組成ガスの分圧は微量ガス分析計(Micropole Sensor,フェラン・サイエンティフィック社、サンディエゴ、カリフォルニア、米国)により、示差式ポンプなしで15mTorrまでは直接測定した。
本実施例はスチレンとアクリロニトリルの重合により形成される16の異なる有機高分子のアレイを合成できる方法を説明する。16の予め画定された領域をその上に有する3cm x 3cmのパイレックス(登録商標)ガラス製の基板を本実施例では用いた。それぞれの画定された領域は3mm x 3mm x 5mmであり、それゆえ各領域の体積は約45mLである。規定の領域の反応物が隣接する領域へはみ出さないことを確かにするためには、35mLの領域を用いるとよい。
この例は異なったアレイを持つゼオライトの可能な合成方法を示している。反応体は16個の前もって定められた区域をもつ9cm×9cmのテフロン(登録商標)基質の所へ運ばれる。その基質を約100℃の密閉容器のなかに置く。基質上の16個の前もって定められた区域の各々は、すべて1cm×1cm×2cmである。反応体は自動ピペットで基質の所へ運ばれる。
この例は噴霧沈積法を用いる酸化銅のアレイの合成法を示している。反応体は16個の前もって定められた区域をもつ1.25cm×1.25cmのMgO基質の所へ運ばれる。反応体は物理的遮蔽技術と噴霧器との組み合わせを用いて薄いフィルムの形で運ばれる。この例で用いた噴霧器はSinitek8700−120MS超音波噴霧器である。水の流れる速さは0.26GPM、周波数は120KHzで、この噴霧器は2インチの錐状噴霧と直径18ミクロンの小滴を発生することができる。
この例は16個の異なった亜鉛珪酸塩リン光体のアレイの可能な合成例を示している。この例では16個の前もって定められた区域をもつ1mm×1mmのパイレックス(登録商標)基質を用いた。各々の前もって定められた区域は100μm×100μm×500μmで、このように各々の前もって定められた区域は約5000ピコリットルとなる。与えられた区域の反応体が隣接の区域に動かないことを保証するために、3000ピコリットルの反応体積が用いられる。
この例は酸化銅材料のアレイの可能な合成法と遮蔽を示している。反応体は256個の前もって定められた区域をもつ1.25cm×1.25cmのMgO基質の所へ運ばれる。MgO基質の1つの側面を粗い面とし、他の側面をきれいに磨いた(1ミクロンのダイヤモンドガラスで)面とする。スパッターした金属酸化物層が良く粘着するためには、表面を極度にクリーンかつなめらかにする必要がある。反応体はスカッター法とフォトリソグラフィー技術の組み合わせを用いて薄いフィルムの形で基質へ運ばれる。フォトレジストは物理的遮蔽として働く。フォトレジストの型はスパッターした材料がどこに沈積し、どこに離昇したかによって決まる。
本発明は単一の支持体上に材料のアレイを並列に堆積し、合成し、スクリーニングする方法及び装置を大きく改良するものである。上記の記載は例示的なものであり、それに限定するものではない。発明の多くの実施態様及び変更はこの開示を見れば当業者にとって明らかである。単なる例として、一定の工程の異なる順序の利用と同様に、さまざまな反応時間、反応温度及び他の反応条件、を利用できる。従って、本発明の範囲は上記の記載から決定されるべきでなく、添付した特許請求の範囲から決定されるべきであり、その請求の範囲に与えられる権利と均等な範囲も含むものである。
Claims (8)
- 材料のアレイを製造及びスクリーニングする方法であって、
支持体上の第一の非生物有機ポリマー及び第二の非生物有機ポリマーを含み、前記第一の非生物有機ポリマーが前記第二の非生物有機ポリマーとは異なっている、アレイを準備することと、
前記第一及び第二の非生物有機ポリマーを含む前記アレイを、熱的性質、機械的性質、形態学的性質、化学的性質、光学的性質、磁気的性質及び電気的性質からなる群より選ばれる性質に関してスクリーニングすることと、
を含み、
前記アレイが、
前記第一の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第一の領域に送り出すこと、
前記第二の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第二の領域に送り出すこと、
開始剤を前記支持体上の前記第一及び第二の領域に送り出すこと、
前記第一の非生物有機ポリマーの送り出された前記第一及び第二モノマーを反応させて前記第一の非生物有機ポリマーを前記支持体上の前記第一の領域で生成させること、並びに、
前記第二の非生物有機ポリマーの送り出された前記第一及び第二モノマーを反応させて前記第二の非生物有機ポリマーを前記支持体上の前記第二の領域で生成させること、
を含む方法によって準備される、方法。 - 前記非生物有機ポリマーが、ポリウレタン、ポリエステル、ポリカーボネイト、ポリエチレンイミン、ポリアセテート、ポリスチレン、ポリアミド、ポリアニリン、ポリアセチレン、ポリピロール、及びこれらのコポリマーからなる群より選ばれる、請求項1に記載の方法。
- 前記第一の非生物有機ポリマーの送り出された前記第一及び第二モノマーを反応させて前記第一の非生物有機ポリマーを前記支持体上の前記第一の領域で生成させることと、前記第二の非生物有機ポリマーの送り出された前記第一及び第二モノマーを反応させて前記第二の非生物有機ポリマーを前記支持体上の前記第二の領域で生成させることとが、同時に起こる、請求項1又は2に記載の方法。
- 前記アレイが、前記支持体の前記第一及び第二の領域における重合の反応条件を独立に制御すること、を更に含む方法によって準備される、請求項1〜3のいずれか一項に記載の方法。
- 反応溶媒、反応温度、反応時間、及び反応を抑制する速度から選ばれる反応条件を、前記支持体の前記領域ごとに変化させる、請求項4に記載の方法。
- 前記第一及び第二の領域に送り出される前記第一モノマーが同一であるが、前記第一モノマーが前記第一及び第二の領域に異なった量で与えられ、
前記第一及び第二の領域に送り出される前記第二モノマーが同一であるが、前記第二モノマーが前記第一及び第二の領域に異なった量で与えられる、
請求項1に記載の方法。 - 前記アレイが、少なくとも10の非生物有機ポリマーを前記支持体の少なくとも10の領域に含み、前記アレイが、
第三の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第三の領域に送り出すこと、
第四の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第四の領域に送り出すこと、
第五の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第五の領域に送り出すこと、
第六の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第六の領域に送り出すこと、
第七の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第七の領域に送り出すこと、
第八の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第八の領域に送り出すこと、
第九の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第九の領域に送り出すこと、並びに、
第十の非生物有機ポリマーの第一モノマー及び第二モノマーを前記支持体上の第十の領域に送り出すこと、
を更に含む方法によって準備される、請求項1又は2に記載の方法。 - 少なくとも10の前記非生物有機ポリマーそれぞれの前記第一モノマーが同一であるが、前記第一モノマーの化学量論が前記支持体の少なくとも10の前記領域間で一定の勾配で変化する、請求項7に記載の方法。
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