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JP2004195340A - Method and apparatus for handling fine particles - Google Patents

Method and apparatus for handling fine particles Download PDF

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JP2004195340A
JP2004195340A JP2002365780A JP2002365780A JP2004195340A JP 2004195340 A JP2004195340 A JP 2004195340A JP 2002365780 A JP2002365780 A JP 2002365780A JP 2002365780 A JP2002365780 A JP 2002365780A JP 2004195340 A JP2004195340 A JP 2004195340A
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fine particles
substrate
handling
ultrasonic
solution
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JP4415139B2 (en
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Jun Aketo
純 明渡
Maxim Lebedev
マキシム レベデフ
Harumichi Sato
治道 佐藤
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National Institute of Advanced Industrial Science and Technology AIST
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    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/06—Fluid handling related problems
    • B01L2200/0647—Handling flowable solids, e.g. microscopic beads, cells, particles
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    • B01L2400/0433—Moving fluids with specific forces or mechanical means specific forces vibrational forces
    • B01L2400/0439—Moving fluids with specific forces or mechanical means specific forces vibrational forces ultrasonic vibrations, vibrating piezo elements
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Abstract

【課題】本発明は、超音波輻射による微粒子の凝集現象とフラットな基板上に展開された液膜の表面張力を利用し、流路やキャビティーなどのガイド無しに、基板上で超音波を用いて微粒子をハンドリングする技術を提供することを目的とする。
【解決手段】本発明の微粒子のハンドリング方法は、溶液と混合された微粒子を基板上に展開し、これに超音波を印加し、微粒子と溶液を搬送、混合、凝集、濃縮又は分離することを特徴とする。また、本発明の微粒子のハンドリング装置は、溶液と混合された微粒子を表面に展開する基板の裏面に超音波発生源を設け、前記基板の裏面側から液体と混合された微粒子に超音波を印加することを特徴とする。
【選択図】 図１An object of the present invention is to utilize an agglomeration phenomenon of fine particles due to ultrasonic radiation and a surface tension of a liquid film spread on a flat substrate to generate ultrasonic waves on a substrate without a guide such as a flow path or a cavity. It is an object of the present invention to provide a technique for handling fine particles using the same.
A method for handling fine particles of the present invention includes developing fine particles mixed with a solution on a substrate, applying ultrasonic waves to the fine particles, and conveying, mixing, aggregating, concentrating, or separating the fine particles and the solution. Features. Further, in the fine particle handling apparatus of the present invention, an ultrasonic wave generating source is provided on the back surface of the substrate that spreads the fine particles mixed with the solution on the surface, and ultrasonic waves are applied to the fine particles mixed with the liquid from the back surface side of the substrate. It is characterized by doing.
[Selection diagram] Fig. 1

Description

【０００１】
【発明の属する技術分野】
本発明は、基板上に展開された大きさが１００μｍ以下の微粒子、薬剤粉末及びＤＮＡ等（本明細書では、これらを総称して単に「微粒子」という。）を基板上で搬送、混合、濃縮、分離する方法及び装置に関する。
【０００２】
【従来の技術】
生物学、医学、薬学の分野では、処理の高速化や機器の携帯性など様々な理由から液中に分散された極微量の試料を非接触に取り扱い、分析・診断する技術が求められている。
従来、液中に分散された微粒子をハンドリングするためにレーザーによる光輻射や加熱による液体流れによる手法が提案されている（従来例１）。
また、マイクロマシニングなどを応用した微小化学分析装置や医療用分析装置では、その携帯性を高めるため分析素子の配置された基板上に被分析試料や薬液をガイドするための微小な流路やキャビティーを設けたカード状の分析装置が提案されている（従来例２）。
【０００３】
【発明が解決しようとする課題】
しかしながら、従来例１のように、熱的な効果を利用した場合、微粒子の搬送応答速度や安定性に問題があり、基板上に展開された薄い液膜内の強い表面張力に保持された大量の微粒子を一括してハンドリングする事は困難で、扱える分量も僅かで実用性に欠けていた。
また、従来例２の場合、微小な流路やキャビティーに付着した薬液やＤＮＡなどの固体の分析試料はクリーニングが容易でなく、使い捨ての機器にならざる得なかった。従って、高度で複雑な分析を行うと高価な物になり、その用途は限定された物になる等の課題があった。
【０００４】
本発明は、従来技術の有する問題点を解決すべく新しい知見に基づきなされたもので、超音波輻射による微粒子の凝集現象とフラットな基板上に展開された液膜の表面張力を利用し、流路やキャビティーなどのガイド無しに、基板上で超音波を用いて微粒子をハンドリングする技術を提供することを目的とする。
【０００５】
【課題を解決するための手段】
まず、本発明の原理について説明する。
容器に入れた液中に分散された微粒子に超音波を照射すると、容器内で形成される超音波定在波節の部分の方が腹の部分より圧力が下がり、結果、液中に分散された微粒子が、節の部分に集まり濃縮される。このことは「超音波輻射圧による微粒子の凝集現象」として知られ文献（応用物理Vol.67，3号，p323-326）にも記載されている。
これに対し、基板上に展開あるいは塗布させた印加超音波の波長以下の薄い液膜中の微粒子への超音波照射の場合、液膜の厚みで微粒子の運動は擬２次元的に拘束され、また、超音波源からの距離がその波長以下であるため、後述するように液中に分散した微粒子は、上記超音波輻射圧を用いた場合と異なり、振動の腹の部分に集まる。この違いは、超音波の近接場効果や液膜の微粒子や基板との間に働く表面張力の効果などが顕著になるためと考えられる。
本発明は、この新しい超音波輻射による微粒子の凝集現象とフラットな基板上に展開された液膜の表面張力を利用し、流路やキャビティーなどのガイド無しに、基板上で超音波を用いて微粒子をハンドリングする技術を提供することを目的とする。
なお、本明細書において「超音波」は、高い周波数をもつ各種の弾性波を総称して超音波といい、およそ１ｋＨｚ以上の周波数の音波をいう。
【０００６】
上記目的を達成するため本発明の微粒子のハンドリング方法は、溶液と混合された微粒子を基板上に展開し、これに超音波を印加し、微粒子と溶液を搬送、混合、凝集、濃縮又は分離することを特徴とする。
また、本発明の微粒子のハンドリング方法は、溶液と微粒子とが混合されて形成する液膜の厚みが印加する超音波の波長あるいはその波長以下であることを特徴とする。
また、本発明の微粒子のハンドリング方法は、溶液と微粒子とが混合されて形成する液膜の厚みが微粒子の粒径の３〜１０倍の範囲であること特徴とする。
また、本発明の微粒子のハンドリング装置は、溶液と混合された微粒子を表面に展開する基板の裏面に超音波発生源を設け、前記基板の裏面側から液体と混合された微粒子に超音波を印加することを特徴とする。
また、本発明の微粒子のハンドリング装置は、超音波発生源として基板の裏面にエアロゾルデポジション法で形成されるＰＺＴ膜から成る圧電素子を用いることを特徴とする。
また、本発明の微粒子のハンドリング装置は、基板裏面に少なくとも２カ所以上の超音波発生源を設け、これらの超音波発生源を順次動作させることを特徴とする。
また、本発明の微粒子のハンドリング装置は、微粒子が１μｍ以上、１００μｍ以下であることを特徴とする。
また、本発明の微粒子のハンドリング装置は、溶液と混合された微粒子に印加される超音波が、１ｋＨｚ以上であることを特徴とする。
また、本発明の微粒子のハンドリング装置は、溶液と微粒子とが混合されて形成する液膜の厚みが１０ｍｍ以下であることを特徴とする。
また、本発明の微粒子のハンドリング装置は、基板の厚みが０.５〜５００μｍの範囲であることを特徴とする。
また、本発明の微粒子のハンドリング装置は、超音波発生源に印加する電圧振幅が３０Ｖ以下であることを特徴とする。
【０００７】
【発明の実施の形態】
以下、本発明による実施の形態を図面に基づき説明する。
〔実施の形態１〕
図１乃至図７は、実施の形態１を示す図である。
図１は、微粒子ハンドリング装置の概略を示す正面断面図であり、左側の図が電源ＯＦＦ時を、右側の図が電源ＯＮ時を示している。
微粒子ハンドリング装置は、以下の手順で作製される。
まず、Ｓｉ基板１をプラズマエッチング（ＩＣＰ−ＲＩＥ：誘導プラズマ結合反応性エッチング）あるいは化学エッチング（異方性エッチング）などで加工し、図１に示すような薄いＳｉ基板の領域２を設け（結果として微小な容器（キャビティー）を構成することになる。）、この領域２の底面に超音波を発生するための超音波発生源３を設ける。
この超音波発生源３は、上部電極４、下部電極５の設けられたＰＺＴなどの圧電素子７を上記基板１裏面の所定の位置に張り付ける。このとき、上記超音波発生発生源３である圧電素子７をエアロゾルデポジション法（例えば、特許公開２００２−２０８７８に開示されている微粒子堆積法）でＰＺＴ微粒子をＰｔなどの下部電極５の設けられたＳｉ基板１に吹きつけ直接形成すると、接着剤などを介さないため、発生した超音波の吸収が最小限に抑えられ、Ｓｉ基板１上に塗布された液膜内に超音波を広い周波数に渡り効率的に伝搬させることが可能となる。
さらに形成するＰＺＴ圧電素子７の厚みの下限は、微粒子をハンドリングするのに必要な超音波の発生パワーからして１μｍ以上、また小型デバイスとして実用に供する観点から駆動電圧を低減するために５０μｍ以下に設定することが望ましい。また、Ｓｉなどできた基板１の厚みは、ＰＺＴ圧電素子７の厚みと同様に、局所的あるは効率的な超音波の印加を考慮し、５００μｍ以下であることが望ましい。
【０００８】
次に、この様に形成された超音波発生源３を設けた基板１に、粒径５００μｍ以下のガラス微粒子８と溶液９を混合したものを塗布あるは滴下し、薄い液膜１０を形成し、前記超音波発生源３の配置された基板１底面から基板１表面に向けて１ｋＨｚ以上の周波数で超音波を発生させると、基板１表面の溶液に分散していた微粒子８は、図２乃至図５に示すように圧電素子が配置され音波振動の腹の部分となる超音波源の中心部に集まり凝集、濃縮される。
【０００９】
図２乃至図５に示す実験例▲１▼〜▲４▼では、微粒子８の粒径は５μｍ、２０μｍ、１２４μｍで、液膜１０の厚みは１〜６ｍｍ、Ｓｉ基板１厚みは６５μｍ、１００μｍ、圧電素子（ＰＺＴ層）７厚みは１０〜１５μｍ、駆動超音波の周波数は、１０ｋＨｚ，１３ｋＨｚ，９６ｋＨｚ，１４４ｋＨｚ，２１４ｋＨｚ、駆動電圧は±１０Ｖ、溶液９の種類は、水、エチレングルコール、パラフィン、シリコンオイルである。このとき液膜１０面は微粒子８との間に働く表面張力により引きずられ微粒子８の凝集に伴い盛り上がり、印加している超音波振動を切ると、溶液９の熱振動や基板１との表面張力により、超音波発生源直下に濃縮、集められた微粒子８は、再び分散することになる。つまり、超音波照射のＯＮ、ＯＦＦにより、この微粒子８の凝集操作は可逆的に行うことが可能である。
また、超音波照射中に凝集した微粒子は、静的に集まったものでなく、液体との間に流れを作っており、動的に動きながら集まったものである。従って、種類の異なる微粒子を混合することも可能であり、さらに微粒子を溶液と混合、反応させることも可能である。
【００１０】
微粒子８の凝集の速度は、圧電素子７に印加する駆動電圧で制御可能で、超音波源のパワー（素子の振幅）の増加に伴って、微粒子８の移動速度が増加することが確認された。また、図２乃至図４の実験▲１▼〜▲３▼にあるように、微粒子８の粒子径、溶液９の種類に関係無く、超音波により凝集操作を実現することができる。尚、このときの照射超音波の周波数は基板１の共振周波数（溶液有り：５ｋＨｚ，溶液無し：２０ｋＨｚ）ではない。
また、微粒子８の凝集の速度は、上記した圧電素子７に印加する駆動電圧の他に、溶液の粘度、あるいは、微粒子の粒径に応じても凝集速度が変化する。 この性質を利用することにより、微粒子の分離、あるいは微粒子と溶液との分離をすることも可能である。
【００１１】
さらに、図５の実験例▲４▼は、超音波の周波数を変化させたときの凝集操作の変化を調べた結果である。１０ｋＨｚ〜２００ｋＨｚにわたり、凝集操作を実現することができた。このとき、上述した▲１▼〜▲４▼の全ての実験において、溶液中の音波波長は、７ｍｍ〜１５０ｍｍで、液膜１０の厚みや実験に用いた基板１に形成されたキャビティーの大きさ以上で、超音波の波長から本発明の液中微粒子の凝集現象は、近接場超音波の効果によるものと考えられ、先述した超音波輻射圧による液中微粒子の凝集現象とは、メカニズムが異なることが確認された。 また、基板振動部分の振幅（ｄ）は、１０ｎｍ（１０ｋＨｚ時）〜２ｎｍ（２１４ｋＨｚ時）と非常に僅かで、単純な基板振動による粒子の凝集でも無く、超音波による効果であることが明らかになった。
【００１２】
尚、確認のために超音波を印加した際の基板１の振動状態をレーザー変位計（小野測器製：ＬＶ−１６１０＆フリンジカウンターＬＶ−０１２０）で計測した結果、図６に示すように超音波印加により粒子の凝集した超音波源中央部で最大変位をする１次の振動モードであった。また、同じ超音波源を設けた基板に液体を除いた状態で微粒子８だけを載せ、超音波を照射したところ、基板１上の微粒子８はその場で振動するだけで、この様な微粒子８の凝集現象は、全く観察されなかった。つまり、本発明の微粒子のハンドリング手法は、従来、ネジ等の微小部品を搬送するのに使われるパーツフィーダーなどの様な振動と重力を用いた原理とは本質的に異なることが確認された。
【００１３】
この実施例では、塗布する溶液９としては自然蒸発、乾燥を防ぐため水、エチレングルコール、パラフィン、シリコンオイルを使ったが、アルコール類などその他の液体でも同様の操作が可能で、用途により適宜選択する。また、超音波により微粒子８に働く力は、粒径に依存して小さくなり、最終的にはブラウン運動のため散乱されハンドリングできなくなる。実験的には０.５μｍ程度の粒子径までは操作できることが確認された。液膜１０の厚みについては、本発明の場合、使用する微粒子８の粒径にも影響されるが、実験的には使用する微粒直径の３〜１０倍程度が好ましい。
尚、液膜１０を形成する液体９に高粘度あるいは表面張力の大きな液体を用いると、重力の影響を無視でき、基板１表面に特別なカバーを掛けなくとも、基板１上に展開された液体９や微粒子８はこぼれ落ちることなく使用することができ、装置が簡便化する利点がある。
【００１４】
また、上記実施例の実験では、基板１にエッチングにより微小なキャビティーを設けたが、これは溶液９をガイドする為の物でなく、溶液９や微粒子８に局所的かつ効率的に超音波を印加するためにＳｉ基板１を薄くし、側壁からの音波の反射を利用するためで、本装置の動作原理からも、これは必須のものでは無い。従って、Ｓｉ基板１上で超音波を効率的に印加するためにエッチングを施し、厚みを薄くする箇所は、液膜１０の塗布される基板１表面に設ける必要は無く、図７に示すように基板１裏面をエッチングし、超音波発生源３である圧電素子７を設けてもよい。つまり、基板１に超音波が印加されていれば、液膜１０中の微粒子８は超音波発生源３近傍に拘束され、微小キャビティーや微小流路などのガイドが必要でなくフラット（平面）な基板１面上で安定した微粒子のハンドリング、分析が可能となる。また、これにより複雑な流路やキャビティーを設ける必要が無く、分析装置のクリーニングが容易になる。
尚、図７の様な構成の場合、圧電膜の形成は従来薄膜技術では困難で、エアロゾルデポジション法により、ノズルからＰＺＴ微粒子を噴射し、局所的なパターニングを行えば容易に作製できる。
【００１５】
〔実施の形態２〕
図８乃び図９は、実施の形態２を示す図である。
実施の形態１の基本操作を基に、図８に示すようにフラットなＳｉ基板１裏面上に超音波発生源３である圧電素子７を複数配列し、これを順次駆動させることで、その表面上に塗布された液膜１０内の微粒子８を搬送することができる。次にその動作を説明する、まず、複数配列された圧電素子７の一つを動作させると、圧電素子７周辺に存在する粒子８は実施の形態１の原理に基づき圧電素子７の近傍に凝集する。次にこの圧電素子７の駆動を停止し、あるいは漸次弱めながら、隣接された圧電素子７を徐々に駆動すると、圧電素子７の近傍に集まっていた微粒子８は、同様の原理で圧電素子７近傍に引き寄せられ、圧電素子７近傍に凝集する。この様な動作を隣接する複数の圧電素子７にわたり順次駆動する事で、結果的に微粒子８は、基板１上に配置された圧電素子７の配列に応じて、移動することができる。
【００１６】
この様な圧電素子７の配列は、従来の微小流路のパターンに対応するもので、搬送、混合、凝集などの操作の必要に応じて配置、大きさを選ぶ。また、微細な超音波源を図９に示すようにマトリックス状に配置し、一筆書きできる形で順次駆動すると、駆動する超音波源の組み合わせにより同一の素子で、基板１上の微粒子８を任意のベクトル方向にハンドリングが可能となり、様々な目的に応じて同装置を安価に提供することができる。尚、超音波源の配列間隔と各超音波源の切り替わり時間は、液体の粘性、液膜の厚み、粒子の大きさ、超音波の周波数、強度に応じて適宜調整する。
【００１７】
【発明の効果】
本発明によれば、基板上に展開された薄い液膜内の強い表面張力に保持された大量の微粒子を一括してハンドリングする事が可能であり、扱える分量も実用上必要とされるに十分である。また、微粒子の搬送応答速度や安定性にも優れている。
また、本発明では、基板表面に微小流路やキャビティーを形成せず非接触で微粒子のハンドリング（搬送、凝集、混合、分散、分離など）が行えるため、液膜、微粒子の接触する表面は、フラットで装置をクリーニングすることが容易になり、また、流路などの固定されたガイドが液膜、微粒子の接触する基板表面に存在しないため、同一の装置で任意の方向への微粒子、液体の搬送、凝集、分散が可能となる。
また、本発明によれば、従来のものに比して操作が容易であり、また低廉なハンドリング装置の提供が可能である。
【図面の簡単な説明】
【図１】本発明の実施の形態１に係る微粒子のハンドリング装置の概略を示す正面断面図である。
【図２】本発明の実施の形態１による実験例１を示すもので、微粒子のハンドリング装置の上面から撮影した写真である。
【図３】本発明の実施の形態１による実験例２を示すもので、微粒子のハンドリング装置の上面から撮影した写真である。
【図４】本発明の実施の形態１による実験例３を示すもので、微粒子のハンドリング装置の上面から撮影した写真である。
【図５】本発明の実施の形態１による実験例４を示すもので、微粒子のハンドリング装置の上面から撮影した写真である。
【図６】本発明の実施の形態１に係る超音波を印加した際の基板の振動状態をレーザー変位計で計測した結果を示す図である。
【図７】基板裏面をエッチングし、該エッチング部に超音波発生源である圧電素子を設けた例を示す正面図である。
【図８】本発明の実施の形態２に係る、フラットな基板裏面上に超音波発生源である圧電素子を複数配列し、これを順次駆動させることで、基板表面上に塗布された液膜内の微粒子を搬送する状態を示す正面図である。
【図９】本発明の実施の形態２に係る、微細な超音波源をマトリックス状に配置した例を示す説明図である。
【符号の説明】
１ 基板
２ 基板の薄い領域
３ 超音波発生源
４ 上部電極
５ 下部電極
７ 圧電素子
８ 微粒子
９ 溶液
１０ 液膜[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention conveys, mixes, and concentrates fine particles, drug powder, DNA, and the like (these are collectively referred to simply as “fine particles”) having a size of 100 μm or less spread on a substrate on the substrate. , Separation method and apparatus.
[0002]
[Prior art]
In the fields of biology, medicine, and pharmacy, there is a need for techniques for analyzing and diagnosing non-contact trace amounts of samples dispersed in liquids for various reasons, such as faster processing and portability of equipment. .
2. Description of the Related Art Conventionally, in order to handle fine particles dispersed in a liquid, there has been proposed a method using light radiation by a laser or a liquid flow by heating (conventional example 1).
In addition, in microchemical analyzers and medical analyzers that apply micromachining, etc., in order to enhance their portability, minute flow paths and cavities for guiding analytes and chemicals are placed on a substrate on which analytical elements are arranged. A card-shaped analyzer provided with a tee has been proposed (conventional example 2).
[0003]
[Problems to be solved by the invention]
However, when the thermal effect is used as in Conventional Example 1, there is a problem in the transport response speed and stability of the fine particles, and a large amount of liquid held by strong surface tension in a thin liquid film spread on the substrate. It was difficult to handle the fine particles in a lump, and the amount that could be handled was small and lacked practicality.
Further, in the case of Conventional Example 2, a solid analytical sample such as a drug solution or DNA attached to a minute flow path or a cavity is not easy to clean, and has to be disposable. Therefore, there is a problem in that an advanced and complicated analysis becomes expensive and its use is limited.
[0004]
The present invention has been made based on new knowledge to solve the problems of the prior art, and utilizes the phenomenon of agglomeration of fine particles by ultrasonic radiation and the surface tension of a liquid film spread on a flat substrate. An object of the present invention is to provide a technique for handling fine particles using ultrasonic waves on a substrate without a guide such as a path or a cavity.
[0005]
[Means for Solving the Problems]
First, the principle of the present invention will be described.
When ultrasonic waves are applied to the fine particles dispersed in the liquid placed in the container, the pressure of the ultrasonic standing node formed in the container is lower than that of the antinode, and as a result, the particles are dispersed in the liquid. The collected fine particles gather at the nodes and are concentrated. This is known as the "aggregation phenomenon of fine particles by ultrasonic radiation pressure" and is described in the literature (Applied Physics Vol. 67, No. 3, p323-326).
On the other hand, in the case of irradiating the fine particles in a thin liquid film having a wavelength equal to or less than the wavelength of the applied ultrasonic wave spread or applied on the substrate, the movement of the fine particles is quasi-two-dimensionally restricted by the thickness of the liquid film, Further, since the distance from the ultrasonic source is equal to or shorter than the wavelength, the fine particles dispersed in the liquid gather at the antinode of the vibration unlike the case where the ultrasonic radiation pressure is used as described later. It is considered that this difference is due to the remarkable effects of the near-field effect of ultrasonic waves and the effect of surface tension acting on the fine particles of the liquid film and the substrate.
The present invention utilizes the new phenomenon of agglomeration of fine particles by ultrasonic radiation and the surface tension of a liquid film spread on a flat substrate, and uses ultrasonic waves on the substrate without a guide such as a flow path or cavity. It is an object of the present invention to provide a technology for handling fine particles.
In this specification, “ultrasonic waves” generally refer to various kinds of elastic waves having a high frequency as ultrasonic waves, and sound waves having a frequency of about 1 kHz or more.
[0006]
In order to achieve the above object, the method for handling fine particles of the present invention is to develop fine particles mixed with a solution on a substrate, apply ultrasonic waves to the fine particles, transport the fine particles and the solution, mix, aggregate, concentrate or separate. It is characterized by the following.
Further, the method for handling fine particles of the present invention is characterized in that the thickness of the liquid film formed by mixing the solution and the fine particles is equal to or less than the wavelength of the applied ultrasonic wave.
Further, the method for handling fine particles of the present invention is characterized in that the thickness of the liquid film formed by mixing the solution and the fine particles is 3 to 10 times the particle diameter of the fine particles.
Further, in the fine particle handling apparatus of the present invention, an ultrasonic wave generating source is provided on the back surface of the substrate that spreads the fine particles mixed with the solution on the surface, and ultrasonic waves are applied to the fine particles mixed with the liquid from the back surface side of the substrate. It is characterized by doing.
Further, the fine particle handling apparatus of the present invention is characterized in that a piezoelectric element made of a PZT film formed on the back surface of the substrate by an aerosol deposition method is used as an ultrasonic wave generating source.
Further, the apparatus for handling fine particles of the present invention is characterized in that at least two or more ultrasonic sources are provided on the back surface of a substrate, and these ultrasonic sources are sequentially operated.
Further, the fine particle handling apparatus of the present invention is characterized in that the fine particles have a size of 1 μm or more and 100 μm or less.
In the fine particle handling apparatus according to the present invention, the ultrasonic wave applied to the fine particles mixed with the solution is 1 kHz or more.
Further, the fine particle handling apparatus of the present invention is characterized in that a liquid film formed by mixing the solution and the fine particles has a thickness of 10 mm or less.
Further, the fine particle handling apparatus of the present invention is characterized in that the thickness of the substrate is in the range of 0.5 to 500 μm.
Further, the fine particle handling apparatus of the present invention is characterized in that the voltage amplitude applied to the ultrasonic wave generating source is 30 V or less.
[0007]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to the drawings.
[Embodiment 1]
1 to 7 show the first embodiment.
FIG. 1 is a front cross-sectional view schematically showing a particle handling apparatus, in which a left-side diagram shows a state when the power is turned off, and a right-side diagram shows a state when the power is turned on.
The particle handling device is manufactured by the following procedure.
First, the Si substrate 1 is processed by plasma etching (ICP-RIE: Inductive Plasma Coupled Reactive Etching) or chemical etching (anisotropic etching) to provide a thin Si substrate region 2 as shown in FIG. A micro-container (cavity) is formed as the above.), And an ultrasonic wave generating source 3 for generating an ultrasonic wave is provided on the bottom surface of the region 2.
The ultrasonic generator 3 attaches a piezoelectric element 7 such as PZT provided with the upper electrode 4 and the lower electrode 5 to a predetermined position on the back surface of the substrate 1. At this time, the piezoelectric element 7 serving as the ultrasonic wave generation source 3 is provided with the lower electrode 5 such as Pt by applying PZT fine particles to the piezoelectric element 7 by an aerosol deposition method (for example, a fine particle deposition method disclosed in Patent Publication 2002-20878). When formed directly by spraying on the Si substrate 1, the absorption of generated ultrasonic waves is minimized because no adhesive or the like is interposed, and the ultrasonic waves are applied to the liquid film applied on the Si substrate 1 at a wide frequency. Propagation can be performed efficiently.
Further, the lower limit of the thickness of the PZT piezoelectric element 7 to be formed is 1 μm or more in view of the generation power of ultrasonic waves necessary for handling fine particles, and 50 μm or less in order to reduce the driving voltage from the viewpoint of practical use as a small device. It is desirable to set to. The thickness of the substrate 1 made of Si or the like is desirably 500 μm or less in consideration of local or efficient application of ultrasonic waves, similarly to the thickness of the PZT piezoelectric element 7.
[0008]
Next, a mixture of glass particles 8 having a particle diameter of 500 μm or less and a solution 9 is applied or dropped onto the substrate 1 provided with the ultrasonic generator 3 thus formed to form a thin liquid film 10. When ultrasonic waves are generated at a frequency of 1 kHz or more from the bottom surface of the substrate 1 on which the ultrasonic wave source 3 is disposed toward the surface of the substrate 1, the fine particles 8 dispersed in the solution on the surface of the substrate 1 are separated as shown in FIGS. As shown in FIG. 5, the piezoelectric elements are arranged and gather at the center of the ultrasonic source, which is the antinode of the sound wave vibration, and are aggregated and concentrated.
[0009]
In the experimental examples (1) to (4) shown in FIGS. 2 to 5, the particle diameter of the fine particles 8 is 5 μm, 20 μm, and 124 μm, the thickness of the liquid film 10 is 1 to 6 mm, and the thickness of the Si substrate 1 is 65 μm and 100 μm. The piezoelectric element (PZT layer) 7 has a thickness of 10 to 15 μm, the driving ultrasonic frequency is 10 kHz, 13 kHz, 96 kHz, 144 kHz, 214 kHz, the driving voltage is ± 10 V, and the type of the solution 9 is water, ethylene glycol, paraffin, Silicon oil. At this time, the surface of the liquid film 10 is dragged by the surface tension acting between the particles 8 and rises with the aggregation of the particles 8. When the applied ultrasonic vibration is cut off, the thermal vibration of the solution 9 and the surface tension with the substrate 1 are reduced. Thus, the fine particles 8 concentrated and collected immediately below the ultrasonic generation source are dispersed again. That is, the aggregation operation of the fine particles 8 can be performed reversibly by turning on and off the ultrasonic irradiation.
In addition, the fine particles aggregated during the ultrasonic irradiation are not collected statically, but form a flow with the liquid, and are collected while moving dynamically. Therefore, it is possible to mix different types of fine particles, and it is also possible to mix and react fine particles with a solution.
[0010]
The speed of aggregation of the microparticles 8 can be controlled by the driving voltage applied to the piezoelectric element 7, and it has been confirmed that the moving speed of the microparticles 8 increases as the power of the ultrasonic source (the amplitude of the element) increases. . In addition, as shown in Experiments (1) and (3) of FIGS. 2 to 4, the aggregation operation can be realized by ultrasonic waves regardless of the particle diameter of the fine particles 8 and the type of the solution 9. The frequency of the irradiation ultrasonic wave at this time is not the resonance frequency of the substrate 1 (5 kHz with solution, 20 kHz without solution).
The aggregation speed of the fine particles 8 varies depending on the viscosity of the solution or the particle diameter of the fine particles, in addition to the driving voltage applied to the piezoelectric element 7 described above. By utilizing this property, it is also possible to separate fine particles or separate fine particles from a solution.
[0011]
Further, the experimental example {circle around (4)} in FIG. 5 is a result of examining a change in the coagulation operation when the frequency of the ultrasonic wave is changed. The coagulation operation was able to be realized over 10 kHz to 200 kHz. At this time, in all the experiments (1) to (4) described above, the sound wave wavelength in the solution was 7 mm to 150 mm, and the thickness of the liquid film 10 and the size of the cavity formed in the substrate 1 used in the experiment were measured. Above, from the wavelength of the ultrasonic wave, the aggregation phenomenon of the fine particles in the liquid of the present invention is considered to be due to the effect of near-field ultrasonic waves, and the aggregation phenomenon of the fine particles in the liquid by the aforementioned ultrasonic radiation pressure has a mechanism. It was confirmed that they were different. In addition, the amplitude (d) of the vibration part of the substrate is as very small as 10 nm (at 10 kHz) to 2 nm (at 214 kHz). became.
[0012]
As a result of measuring the vibration state of the substrate 1 when applying ultrasonic waves for confirmation with a laser displacement meter (LV-1610 & Fringe Counter LV-0120 manufactured by Ono Sokki), as shown in FIG. This was a primary vibration mode in which the maximum displacement occurred at the center of the ultrasonic source in which particles were aggregated by application. When only the fine particles 8 are placed on the substrate provided with the same ultrasonic source and the liquid is removed, and the ultrasonic waves are irradiated, the fine particles 8 on the substrate 1 only vibrate in place, and the fine particles 8 Was not observed at all. That is, it has been confirmed that the method of handling fine particles according to the present invention is essentially different from the principle of using vibration and gravity, such as a parts feeder used for transporting minute parts such as screws.
[0013]
In this example, water, ethylene glycol, paraffin, and silicone oil were used as the solution 9 to be applied to prevent spontaneous evaporation and drying. However, the same operation can be performed with other liquids such as alcohols, and the liquid is appropriately used depending on the application. select. In addition, the force acting on the fine particles 8 by the ultrasonic waves becomes small depending on the particle size, and eventually becomes scattered due to Brownian motion and cannot be handled. It has been experimentally confirmed that operation can be performed up to a particle diameter of about 0.5 μm. In the present invention, the thickness of the liquid film 10 is affected by the particle size of the fine particles 8 used, but is preferably about 3 to 10 times the fine particle diameter used experimentally.
If a liquid having a high viscosity or a large surface tension is used as the liquid 9 for forming the liquid film 10, the influence of gravity can be ignored, and the liquid developed on the substrate 1 can be dispensed with without a special cover on the surface of the substrate 1. 9 and the fine particles 8 can be used without spilling, and there is an advantage that the apparatus is simplified.
[0014]
Further, in the experiment of the above embodiment, a minute cavity was formed by etching in the substrate 1, but this is not for guiding the solution 9, but for locally and efficiently applying ultrasonic waves to the solution 9 and the fine particles 8. This is because the thickness of the Si substrate 1 is reduced to apply the reflection, and the reflection of the sound wave from the side wall is used. This is not essential also from the operation principle of the present apparatus. Therefore, it is not necessary to provide an etching on the Si substrate 1 in order to efficiently apply ultrasonic waves and to reduce the thickness thereof on the surface of the substrate 1 on which the liquid film 10 is applied, as shown in FIG. The back surface of the substrate 1 may be etched to provide the piezoelectric element 7 as the ultrasonic wave generating source 3. That is, if the ultrasonic wave is applied to the substrate 1, the fine particles 8 in the liquid film 10 are confined in the vicinity of the ultrasonic wave generating source 3, and a flat (planar) without the need for a guide such as a microcavity or a microchannel. This enables stable handling and analysis of fine particles on the surface of a simple substrate. This also eliminates the need to provide a complicated flow path or cavity, and facilitates cleaning of the analyzer.
In the case of the configuration as shown in FIG. 7, it is difficult to form the piezoelectric film by the conventional thin film technology. The piezoelectric film can be easily manufactured by spraying PZT fine particles from a nozzle by an aerosol deposition method and performing local patterning.
[0015]
[Embodiment 2]
8 and 9 show the second embodiment.
Based on the basic operation of the first embodiment, as shown in FIG. 8, a plurality of piezoelectric elements 7 as the ultrasonic wave generating sources 3 are arranged on the back surface of the flat Si substrate 1 and sequentially driven to drive the piezoelectric elements 7 so that the surface The fine particles 8 in the liquid film 10 applied thereon can be transported. Next, the operation will be described. First, when one of the plurality of arranged piezoelectric elements 7 is operated, the particles 8 present around the piezoelectric element 7 aggregate in the vicinity of the piezoelectric element 7 based on the principle of the first embodiment. I do. Next, when the driving of the piezoelectric element 7 is stopped or gradually weakened while gradually weakening the adjacent piezoelectric element 7, the fine particles 8 gathered in the vicinity of the piezoelectric element 7 are moved to the vicinity of the piezoelectric element 7 by the same principle. And aggregates near the piezoelectric element 7. By sequentially driving such an operation over a plurality of adjacent piezoelectric elements 7, as a result, the fine particles 8 can move according to the arrangement of the piezoelectric elements 7 arranged on the substrate 1.
[0016]
Such an arrangement of the piezoelectric elements 7 corresponds to a pattern of a conventional microchannel, and the arrangement and size thereof are selected according to the necessity of operations such as conveyance, mixing, and aggregation. Also, when the fine ultrasonic sources are arranged in a matrix as shown in FIG. 9 and sequentially driven in a form that can be drawn with one stroke, the fine particles 8 on the substrate 1 can be arbitrarily changed by the combination of the ultrasonic sources to be driven. , And can be provided at low cost for various purposes. Note that the arrangement interval of the ultrasonic sources and the switching time of each ultrasonic source are appropriately adjusted according to the viscosity of the liquid, the thickness of the liquid film, the size of the particles, the frequency and the intensity of the ultrasonic wave.
[0017]
【The invention's effect】
According to the present invention, it is possible to collectively handle a large amount of fine particles held at a strong surface tension in a thin liquid film spread on a substrate, and the amount that can be handled is sufficient for practical use. It is. It is also excellent in the response speed and stability of transporting fine particles.
In addition, in the present invention, fine particles can be handled (conveyed, aggregated, mixed, dispersed, separated, etc.) without forming a microchannel or a cavity on the substrate surface. It is easy to clean the device with a flat surface, and there is no fixed guide such as a flow path on the surface of the substrate where the liquid film and the fine particles come into contact. Transport, agglomeration and dispersion.
Further, according to the present invention, it is possible to provide an inexpensive handling device which is easier to operate than conventional ones.
[Brief description of the drawings]
FIG. 1 is a front sectional view schematically showing a fine particle handling apparatus according to Embodiment 1 of the present invention.
FIG. 2 shows Experimental Example 1 according to Embodiment 1 of the present invention, and is a photograph taken from the upper surface of a device for handling fine particles.
FIG. 3 shows Experimental Example 2 according to Embodiment 1 of the present invention, and is a photograph taken from the upper surface of a device for handling fine particles.
FIG. 4 shows Experimental Example 3 according to Embodiment 1 of the present invention, and is a photograph taken from the upper surface of a device for handling fine particles.
FIG. 5 is a photograph of Experimental Example 4 according to Embodiment 1 of the present invention, which is taken from the upper surface of the device for handling fine particles.
FIG. 6 is a diagram showing a result of measuring the vibration state of the substrate when applying an ultrasonic wave according to the first embodiment of the present invention with a laser displacement meter.
FIG. 7 is a front view showing an example in which the back surface of the substrate is etched and a piezoelectric element serving as an ultrasonic wave generating source is provided in the etched portion.
FIG. 8 is a view showing a liquid film applied on the surface of a flat substrate according to a second embodiment of the present invention, in which a plurality of piezoelectric elements, which are ultrasonic wave sources, are arranged on a flat back surface of the flat substrate and sequentially driven. FIG. 4 is a front view showing a state of transporting fine particles inside.
FIG. 9 is an explanatory diagram showing an example in which fine ultrasonic sources are arranged in a matrix according to the second embodiment of the present invention.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Substrate 2 Thin area of substrate 3 Ultrasonic wave generator 4 Upper electrode 5 Lower electrode 7 Piezoelectric element 8 Fine particle 9 Solution 10 Liquid film

Claims (11)

溶液と混合された微粒子を基板上に展開し、これに超音波を印加し、微粒子と溶液を搬送、混合、凝集、濃縮又は分離することを特徴とする微粒子のハンドリング方法。 A method of handling fine particles, comprising: developing fine particles mixed with a solution on a substrate; applying ultrasonic waves to the fine particles; and conveying, mixing, aggregating, concentrating, or separating the fine particles and the solution. 溶液と微粒子とが混合されて形成する液膜の厚みが印加する超音波の波長あるいはその波長以下であることを特徴とする請求項１記載の超音波微粒子ハンドリング方法2. The ultrasonic particle handling method according to claim 1, wherein the thickness of the liquid film formed by mixing the solution and the particles is equal to or less than the wavelength of the applied ultrasonic wave. 溶液と微粒子とが混合されて形成する液膜の厚みが微粒子の粒径の３〜１０倍の範囲であること特徴とする請求項１に記載の微粒子のハンドリング方法。The method for handling fine particles according to claim 1, wherein the thickness of the liquid film formed by mixing the solution and the fine particles is in the range of 3 to 10 times the particle diameter of the fine particles. 溶液と混合された微粒子を表面に展開する基板の裏面に超音波発生源を設け、前記基板の裏面側から液体と混合された微粒子に超音波を印加することを特徴とする微粒子のハンドリング装置。An apparatus for handling fine particles, comprising: an ultrasonic wave generating source provided on a back surface of a substrate on which fine particles mixed with a solution are spread on a surface, and applying ultrasonic waves to the fine particles mixed with a liquid from the rear surface side of the substrate. 超音波発生源として基板の裏面にエアロゾルデポジション法で形成されるＰＺＴ膜から成る圧電素子を用いることを特徴とする請求項４記載の微粒子のハンドリング装置。5. The apparatus for handling fine particles according to claim 4, wherein a piezoelectric element made of a PZT film formed on the back surface of the substrate by an aerosol deposition method is used as an ultrasonic wave generating source. 基板裏面に少なくとも２カ所以上の超音波発生源を設け、これらの超音波発生源を順次動作させることを特徴とする請求項４又は５記載の微粒子のハンドリング装置。6. The apparatus for handling fine particles according to claim 4, wherein at least two or more ultrasonic sources are provided on the back surface of the substrate, and these ultrasonic sources are sequentially operated. 微粒子が１μｍ以上、１００μｍ以下であることを特徴とする請求項４乃至請求項６のいずれか１項に記載の微粒子のハンドリング装置。The device for handling fine particles according to any one of claims 4 to 6, wherein the fine particles have a size of 1 µm or more and 100 µm or less. 溶液と混合された微粒子に印加される超音波が、１ｋＨｚ以上であることを特徴とする請求項４乃至請求項７のいずれか１項に記載の微粒子のハンドリング装置。The apparatus for handling fine particles according to any one of claims 4 to 7, wherein the ultrasonic wave applied to the fine particles mixed with the solution is 1 kHz or more. 溶液と微粒子とが混合されて形成する液膜の厚みが１０ｍｍ以下であることを特徴とする請求項４乃至請求項８のいずれか１項に記載の微粒子のハンドリング装置。The device for handling fine particles according to any one of claims 4 to 8, wherein a thickness of a liquid film formed by mixing the solution and the fine particles is 10 mm or less. 基板の厚みが０.５〜５００μｍの範囲であることを特徴とする請求項１乃至請求項９のいずれか４項に記載の微粒子のハンドリング装置。The apparatus for handling fine particles according to any one of claims 1 to 9, wherein the thickness of the substrate is in a range of 0.5 to 500 µm. 超音波発生源に印加する電圧振幅が３０Ｖ以下であることを特徴とする請求項４乃至請求項１０のいずれか１項に記載の微粒子のハンドリング装置。The apparatus for handling fine particles according to any one of claims 4 to 10, wherein a voltage amplitude applied to the ultrasonic generator is 30 V or less.
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