JP6619873B2 - Pullable flexible ultra-phophophobic film, method for producing the same, and method for non-destructive transfer of droplets - Google Patents
Pullable flexible ultra-phophophobic film, method for producing the same, and method for non-destructive transfer of droplets Download PDFInfo
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- 238000000034 method Methods 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 238000012546 transfer Methods 0.000 title claims description 10
- 230000001066 destructive effect Effects 0.000 title description 17
- 239000002086 nanomaterial Substances 0.000 claims description 44
- -1 fluorocarbon compound Chemical class 0.000 claims description 16
- 239000000839 emulsion Substances 0.000 claims description 13
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 12
- 230000002209 hydrophobic effect Effects 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 11
- QRPMCZNLJXJVSG-UHFFFAOYSA-N trichloro(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10-henicosafluorodecyl)silane Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)[Si](Cl)(Cl)Cl QRPMCZNLJXJVSG-UHFFFAOYSA-N 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 9
- 238000003682 fluorination reaction Methods 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- 239000013013 elastic material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004033 plastic Substances 0.000 claims description 7
- 229920003023 plastic Polymers 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 6
- 238000004528 spin coating Methods 0.000 claims description 6
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 238000001338 self-assembly Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 229920002943 EPDM rubber Polymers 0.000 claims description 2
- 229920000459 Nitrile rubber Polymers 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000008280 blood Substances 0.000 claims description 2
- 210000004369 blood Anatomy 0.000 claims description 2
- 229920001971 elastomer Polymers 0.000 claims description 2
- 239000008267 milk Substances 0.000 claims description 2
- 210000004080 milk Anatomy 0.000 claims description 2
- 235000013336 milk Nutrition 0.000 claims description 2
- 210000002381 plasma Anatomy 0.000 claims description 2
- 229920001084 poly(chloroprene) Polymers 0.000 claims description 2
- 229920002857 polybutadiene Polymers 0.000 claims description 2
- 239000005060 rubber Substances 0.000 claims description 2
- 230000003075 superhydrophobic effect Effects 0.000 claims 3
- 238000007740 vapor deposition Methods 0.000 claims 2
- 239000013536 elastomeric material Substances 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000001723 curing Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005672 electromagnetic field Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000010336 energy treatment Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
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Description
本発明は、引張り可能な可撓超疎液性フィルム、その製造方法及び液滴の非破壊性移動方法に関し、微小液滴操作制御の技術分野に属する。 The present invention relates to a pullable flexible ultra-phophophobic film, a manufacturing method thereof, and a non-destructive transfer method of droplets, and belongs to the technical field of micro droplet operation control.
近年、表面上で液滴を操作する平面マイクロ流体チップは、大きな関心を集めている。平面マイクロ流体チップは、従来のチャネルマイクロ流体チップに比べ、チャネルマイクロ流体チップのような小型化、集積化、試薬消費量が少ない、及び分析速度が速いなどの利点に加えて、例えば、液滴に直接な接触が容易であること、固体サンプルの取り扱い及び液滴アレイの生成に便利であること、固体粒子及び気泡によるマイクロチャネルの目詰まりの恐れがないことなどの、チャネルマイクロ流体チップの備えていない利点を多く持っている。 In recent years, planar microfluidic chips that manipulate droplets on surfaces have gained great interest. The planar microfluidic chip has advantages such as downsizing, integration, low reagent consumption, and high analysis speed as compared with the conventional channel microfluidic chip, as compared with the conventional channel microfluidic chip. Equipped with a channel microfluidic chip, such as easy direct contact with the sample, convenient for handling solid samples and generating droplet arrays, and no risk of clogging of the microchannels due to solid particles and bubbles Not have a lot of benefits.
しかしながら、従来の連続流体により駆動されるチャネルマイクロ流体チップに比べ、現在の表面マイクロ流体チップは、効果的な液滴操作方法がまだ不十分である。近年、一部の光制御、電磁場制御、機械的振動制御及び音場励起制御などの表面微小液滴操作技術の開発により、チャネルマイクロ流体技術の欠点の一部が克服されたが、これらの液滴操作技術は、液滴の成分、マイクロ流体液滴サンプルの伝送経路及び方向などが大きく制限される。現在、主流となっている平面液滴操作方法は、エレクトロウェッティングによって液滴の運動を駆動させ、基板に電極アレイを埋め込み、異なる電極に交互に電圧を印加し、液滴を駆動するものである。電極アレイの埋め込み及び高い駆動電圧が要求されるため、システム集積が困難である。 However, compared to conventional channel microfluidic chips driven by continuous fluids, current surface microfluidic chips still lack effective droplet manipulation methods. In recent years, the development of surface microdroplet manipulation techniques such as some light control, electromagnetic field control, mechanical vibration control and sound field excitation control has overcome some of the drawbacks of channel microfluidic technology. Drop manipulation techniques are severely limited in droplet composition, microfluidic droplet sample transmission path and direction, and the like. At present, the mainstream planar droplet operation method is to drive the droplet by driving the droplet movement by electrowetting, embedding the electrode array on the substrate, and alternately applying a voltage to different electrodes. is there. System integration is difficult because the electrode array is embedded and a high drive voltage is required.
本発明は、上記のような技術的課題を解決するために、引張り可能な可撓超疎液性フィルム及びその製造方法を提供することを目的とするものである。当該フィルムを利用することによって、液滴の非破壊性移動を実現することができる。 In order to solve the technical problems as described above, it is an object of the present invention to provide a flexible super lyophobic film that can be pulled and a method for producing the same. By using the film, non-destructive movement of droplets can be realized.
また、本発明は、前記引張り可能な可撓超疎液性フィルムを使用した液滴の非破壊性移動方法を提供することを目的とするものでもある。当該方法を利用することによって、任意の成分及び大きさの微小液滴の伝送を実現でき、微小液滴に対する処理を一切することなく、従来の微小液滴操作制御技術にある欠点を克服でき、微小液滴操作制御技術の適用範囲を広げることができる。 Another object of the present invention is to provide a non-destructive transfer method of droplets using the pullable flexible ultra-phophophobic film. By utilizing this method, it is possible to realize transmission of microdroplets of arbitrary components and sizes, and overcoming the drawbacks of conventional microdroplet operation control technology without any processing on microdroplets, The application range of the micro droplet operation control technology can be expanded.
上記の目的を達成するためには、本発明は、引張り可能な可撓超疎液性フィルムの製造方法を提供する。該製造方法のプロセスは、図1に示されたように、具体的には、
(1)オーバーハングマイクロ・ナノ構造を有するテンプレートに対しフッ素化修飾を行い、硬化性弾性材料を流れ込むステップ、
(2)硬化した後に、前記硬化性弾性材料をオリジナルテンプレートから剥離し、オーバーハングマイクロ・ナノ構造に対応するマイクロ・ナノ構造を有する中間体を得るステップ、
(3)前記中間体のオーバーハングマイクロ・ナノ構造に対応するマイクロ・ナノ構造を有する層の表面にプラスチックエマルジョンをスピンコートするステップ、
(4)スピンコートされたプラスチックエマルジョンを硬化させ、フィルムを形成するステップ、及び
(5)硬化したフィルムを剥離し、フッ素化修飾を行い、前記引張り可能な可撓超疎液性フィルムを得るステップ
を含む。
In order to achieve the above object, the present invention provides a method for producing a pullable flexible ultra-phobic film. As shown in FIG. 1, specifically, the process of the manufacturing method is as follows.
(1) A step of performing fluorination modification on a template having an overhanging micro / nanostructure and flowing a curable elastic material;
(2) after curing, peeling the curable elastic material from the original template to obtain an intermediate having a micro-nano structure corresponding to an overhanging micro-nano structure;
(3) spin-coating a plastic emulsion on the surface of the layer having a micro / nano structure corresponding to the overhanging micro / nano structure of the intermediate;
(4) a step of curing the spin-coated plastic emulsion to form a film; and (5) a step of peeling the cured film and performing fluorination modification to obtain the pullable flexible ultra-phophophobic film. including.
前記製造方法において、オーバーハングマイクロ・ナノ構造を有する超疎液性表面テンプレートは、ドライエッチングにより作製されてもよく、又はウェットエッチングによりシリコン基板上に作製されてもよい。好ましくは、前記オーバーハングマイクロ・ナノ構造は、T形、逆台形、球状、釘状、傘状又はキノコ状などである。 In the manufacturing method, the super-lyophobic surface template having an overhanging micro / nano structure may be produced by dry etching or may be produced on a silicon substrate by wet etching. Preferably, the overhanging micro / nanostructure is T-shaped, inverted trapezoidal, spherical, nail-shaped, umbrella-shaped or mushroom-shaped.
前記製造方法において、好ましくは、ステップ(1)において、前記フッ素化修飾は、
オリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面を化学気相蒸着プロセスによって加熱処理して、プラズマ状態のフッ化炭素化合物ガス源でオーバーハングマイクロ・ナノ構造の各々の方向に蒸着を行い、オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップ、或いは
単分子自己組織化プロセスによってオリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面において化学反応を起こさせ、オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップを含み、
より好ましくは、前記疎水処理に用いられた試薬(即ち、フッ化炭素化合物)は、トリメチルクロロシラン(TMCS)、ヘキサメチルジシラザン(HMDS)、及びパーフルオロデシルトリクロロシラン(PFTS)などの低表面エネルギーのフッ素含有試薬の1種又は複数種の組み合わせを含む。
In the production method, preferably, in step (1), the fluorination modification is performed by:
The surface of the overhanging micro / nanostructure of the original template is heat-treated by a chemical vapor deposition process, and deposition is performed in each direction of the overhanging micro / nanostructure with a fluorocarbon compound gas source in a plasma state. Create a hydrophobic fluorocarbon coating on the surface of the micro / nanostructure, or cause a chemical reaction on the surface of the overhanging micro / nanostructure of the original template by a single molecule self-assembly process. Generating a hydrophobic fluorocarbon compound coating on the surface of the nanostructure;
More preferably, the reagent used for the hydrophobic treatment (that is, the fluorocarbon compound) is a low surface energy such as trimethylchlorosilane (TMCS), hexamethyldisilazane (HMDS), and perfluorodecyltrichlorosilane (PFTS). Or a combination of a plurality of fluorine-containing reagents.
前記製造方法において、好ましくは、ステップ(1)において、前記硬化性弾性材料は、ポリジメチルシロキサン、エチレン−プロピレン−ジエン三元共重合ゴム、ニトリル・ブタジエン・ゴム、シスポリブタジエンゴム、及びクロロプレン・ゴムの1種又は複数種の組み合わせを含む。 In the manufacturing method, preferably, in step (1), the curable elastic material is polydimethylsiloxane, ethylene-propylene-diene terpolymer rubber, nitrile-butadiene rubber, cis-polybutadiene rubber, and chloroprene rubber. A combination of one or more of the above.
前記製造方法において、ステップ(2)と(4)において、成膜方法は、低温硬化であってもよく、硬化温度は、典型的に5℃未満である。 In the manufacturing method, in steps (2) and (4), the film forming method may be low temperature curing, and the curing temperature is typically less than 5 ° C.
前記製造方法において、好ましくは、プラスチックエマルジョンをスピンコートする際にスピンコーターの回転数を制御し、異なる回転数で厚さの異なる超疎液性フィルムを得ることとなる。ステップ(3)において、前記スピンコートの回転数を50rpm〜2000rpmとなるように制御する。 In the above production method, preferably, the spin coater is rotated at the time of spin coating with the plastic emulsion to obtain super-lyophobic films having different thicknesses at different rotational speeds. In step (3), the rotational speed of the spin coating is controlled to be 50 rpm to 2000 rpm.
前記製造方法において、好ましくは、ステップ(3)において、前記プラスチックエマルジョンがEVAエマルジョン又はポリプロピレンエマルジョンなどである。 In the manufacturing method, preferably, in step (3), the plastic emulsion is an EVA emulsion or a polypropylene emulsion.
前記製造方法において、好ましくは、ステップ(5)において、前記フッ素化修飾は、
オリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面を化学気相蒸着プロセスによって加熱処理して、プラズマ状態のフッ化炭素化合物ガス源でオーバーハングマイクロ・ナノ構造の各々の方向に蒸着を行い、オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップ、或いは
単分子自己組織化プロセスによってオリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面において化学反応を起こさせ、オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップを含み、
より好ましくは、前記フッ素化修飾に用いられた試薬(即ち、フッ化炭素化合物)は、トリメチルクロロシラン(TMCS)、ヘキサメチルジシラザン(HMDS)、及びパーフルオロデシルトリクロロシラン(PFTS)などの低表面エネルギーのフッ素含有試薬の1種又は複数種の組み合わせを含む。
In the production method, preferably, in step (5), the fluorination modification is performed by:
The surface of the overhanging micro / nanostructure of the original template is heat-treated by a chemical vapor deposition process, and deposition is performed in each direction of the overhanging micro / nanostructure with a fluorocarbon compound gas source in a plasma state. Create a hydrophobic fluorocarbon coating on the surface of the micro / nanostructure, or cause a chemical reaction on the surface of the overhanging micro / nanostructure of the original template by a single molecule self-assembly process. Producing a hydrophobic fluorocarbon compound coating on the surface of the nanostructure;
More preferably, the reagent (ie, fluorocarbon compound) used for the fluorination modification is a low surface such as trimethylchlorosilane (TMCS), hexamethyldisilazane (HMDS), and perfluorodecyltrichlorosilane (PFTS). Includes one or more combinations of energetic fluorine-containing reagents.
また、本発明は、前記製造方法により製造された引張り可能な可撓超疎液性フィルムを提供する。該引張り可能な可撓超疎液性フィルムは、優れた可撓性及び引張り性を有し、大きく湾曲する又は引っ張ることができる。 Moreover, this invention provides the flexible super-liquidphobic film which can be pulled | pulled manufactured by the said manufacturing method. The pullable flexible ultra-phophophobic film has excellent flexibility and tensile properties and can be greatly bent or pulled.
また、本発明は、
液滴を前記引張り可能な可撓超疎液性フィルムの表面に置くステップ1、
もう一枚の引張り可能な可撓超疎液性フィルムの表面を前記液滴に接触させることで、前記液滴を捕獲して移動させるステップ2、及び
マイクロ・ナノ構造のピッチを増加させ、固液接触面積を減らし、前記液滴を前記引張り可能な可撓超疎液性フィルムの表面から落下させ、移動を終了するステップ3を含む液滴の非破壊性移動方法を提供する。
The present invention also provides:
Placing a droplet on the surface of the pullable flexible ultraphobic film 1,
The surface of another pullable flexible ultraphobic film is brought into contact with the droplet to capture and move the droplet, and to increase the pitch of the micro / nanostructure and A liquid non-destructive transfer method comprising the step 3 of reducing the liquid contact area, dropping the liquid drop from the surface of the pullable flexible ultra-phophophobic film, and terminating the movement is provided.
該方法は、外部からの、例えば光、電磁場、機械的振動及び音場励起などのエネルギーをインプットすることなく、液滴の非破壊性移動を実現できる。更に、液滴の成分、マイクロ流体液滴サンプルの伝送経路及び方向などについても特に限定することなく、どの液滴に対しても有効である。 The method can realize non-destructive movement of a droplet without inputting external energy such as light, electromagnetic field, mechanical vibration and sound field excitation. Furthermore, the composition of the droplet, the transmission path and direction of the microfluidic droplet sample are not particularly limited, and the present invention is effective for any droplet.
本発明により提供される液滴の非破壊性移動は、各種異なる種類及び特性の液滴又はそれらの混合物に適用される。好ましくは、前記液滴は、種類及び特性が異なる液滴、異なる液滴の混合物若しくは液滴と固体粒子との混合物を含む。より好ましくは、前記液体は、水溶液、牛乳、血液、血漿、及び生化学試薬のうちの1種又は複数種の組み合わせを含む。 The non-destructive transfer of droplets provided by the present invention applies to a variety of different types and properties of droplets or mixtures thereof. Preferably, the droplets include droplets of different types and characteristics, a mixture of different droplets or a mixture of droplets and solid particles. More preferably, the liquid includes one or more combinations of aqueous solutions, milk, blood, plasma, and biochemical reagents.
前記移動方法において、移動の過程には、超疎液性フィルムが良好な柔軟性と良好な引張り性とを有する特徴を利用して、引っ張ることによって液滴と表面との接触面積及び粘着力を変化させ、液滴の非破壊性移動を実現することができる。また、湾曲することによって表面の曲率を減少させ、液滴と表面との接触面積及び粘着力を低減させて、液滴の非破壊性移動を実現することもできる。即ち、好ましくは、ステップ3において、前記引張り可能な可撓超疎液性フィルムを引っ張る又は湾曲することによってマイクロ・ナノ構造のピッチの増加を実現することができる。 In the moving method, in the moving process, by utilizing the characteristics that the super-lyophobic film has good flexibility and good tensile properties, the contact area and adhesive force between the droplet and the surface are reduced by pulling. To achieve non-destructive movement of the droplets. In addition, the curvature of the surface can be reduced by bending, the contact area between the droplet and the surface and the adhesive force can be reduced, and non-destructive movement of the droplet can be realized. That is, preferably, in step 3, an increase in the pitch of the micro / nano structure can be realized by pulling or bending the pullable flexible ultra-lyophobic film.
いかなる液体に対しても低ぬれ性、低粘着特性を示す超疎液性表面は、表面マイクロ流体液滴操作に理想的である。本発明は、微小電気機械システム(MEMS)加工技術に基づき、特殊なオーバーハング微小構造による超疎液性表面材料を開発した。該表面は、概ねいかなる液体に対しても良好な低ぬれ特性を示すだけでなく、良好な柔軟性と引張り可能な特性とを有するため、表面の引張り、湾曲などの操作によって局所の固液接触面積と曲率とを変化させることができ、表面の液滴に対する粘着力を調節して液滴の非破壊性伝送を実現できる。 A super-lyophobic surface that exhibits low wettability and low adhesion properties to any liquid is ideal for surface microfluidic droplet manipulation. The present invention has developed a super-lyophobic surface material with a special overhanging microstructure based on micro-electromechanical system (MEMS) processing technology. The surface not only exhibits good low-wetting properties to almost any liquid, but also has good flexibility and pullable properties, so that the surface solid-liquid contact can be achieved by operations such as surface pulling and bending. The area and the curvature can be changed, and the non-destructive transmission of the droplet can be realized by adjusting the adhesion force of the surface to the droplet.
本発明の技術内容は、ダブルソフトコピープロセスと低表面エネルギー処理とを組み合わせることにより、表面のマイクロ・ナノ構造が制御可能であり、低ぬれ特性に優れた超疎液性表面を得た。該超疎液性表面の良好な柔軟性及び引張り性を利用し、表面の引張り、湾曲などの操作によって局所の固液接触面積と曲率とを変化させることができ、表面の液滴に対する粘着力を調節して液滴の非破壊性移動及び伝送を実現できる。本発明の技術内容は、従来の微小液滴操作制御技術の欠点を克服し、微小液滴に対する処理を一切することなく、任意の成分及び大きさの微小液滴の伝送を実現でき、微小液滴操作制御技術の適用範囲を広げることができる。 The technical content of the present invention is to combine a double soft copy process and low surface energy treatment to control the surface micro / nano structure, and to obtain a super-lyophobic surface with excellent low wetting characteristics. Utilizing the good flexibility and tensile properties of the super-liquidphobic surface, the local solid-liquid contact area and curvature can be changed by operations such as surface tension and curvature, and the adhesive force to the surface droplets Can be adjusted to achieve non-destructive movement and transmission of the droplets. The technical content of the present invention overcomes the shortcomings of the conventional microdroplet manipulation control technology and can realize the transmission of microdroplets of any component and size without any processing on the microdroplets. The application range of the droplet operation control technology can be expanded.
本発明の構成要件、目的及び有益な効果をより明確に把握するためには、本発明の技術内容を以下に詳細に説明するが、本発明の実施可能な範囲を限定するものであると理解されるべきではない。
<実施例1>
In order to more clearly grasp the configuration requirements, purpose, and beneficial effects of the present invention, the technical contents of the present invention will be described in detail below, but it is understood that the scope of the present invention is limited. Should not be done.
<Example 1>
本実施例は、引張り可能な可撓超疎液性フィルムの製造方法を提供するものであり、以下のステップを含む。
(1)T型マイクロ・ナノ構造を有するオリジナルテンプレートを洗浄し、干燥させた後に、ホットプレート上に置いた。ホットプレートの温度は、150℃に設定した。テンプレートの隣に清潔なスライドガラスを一枚置いておき、3分間予熱した。パーフルオロデシルトリクロロシラン(PFTS)を取り出し、使い捨てピペットを用いてホットプレート上のスライドに2滴を滴下し、ガラスディッシュでホットプレート上のオリジナルテンプレートの表面を被せた。最も高い疎水効果を得るために、ホットプレートで4分間加熱した。
(2)被せたガラスディッシュを外し、予め調製した硬化性弾性材料であるポリジメチルシロキサン(PDMS)を培養皿に注ぎ、80℃の真空乾燥器に入れて、真空雰囲気で2時間焼成し、硬化性弾性材料PDMSを硬化させた。硬化性弾性材料PDMSを剥離した後に、表面にT型マイクロ・ナノ構造を有する中間体が得られた。
(3)表面にT型マイクロ・ナノ構造を有するPDMS中間体を、微小構造面を上にするようにスピンコーターにセットして、液状EVAエマルジョンを中間体の表面に流れ込み、回転数を50rpm〜2000rpmの範囲とし、所望の厚さに応じて異なるスピンコート速度を設定することができ、例えば100rpmの場合、厚さが約160μmであり、300rpmの場合、厚さが約80μmである。
(4)スピンコートした後のEVAエマルジョンをPDMS中間体とともに取り出し、−4℃以下の低温雰囲気に置いて硬化させた。硬化時間はEVAエマルジョンの厚さに従って増加する。硬化後、T型マイクロ・ナノ構造を持つPDMS中間体から剥離し、表面にT型マイクロ・ナノ構造を有するEVAフィルムが得られた。
(5)T型マイクロ・ナノ構造を有するEVAフィルムを、その両端が支えられて吊るすようにホットプレートにセットした。ホットプレートの温度は、70℃に設定した。フィルムの隣に清潔なスライドガラスを一枚置いておき、3分間予熱した。使い捨てピペットを用いてパーフルオロデシルトリクロロシラン(PFTS)をホットプレート上のスライドガラスに数滴を滴下し、ガラスディッシュでホットプレートを上から被せた。最も高い疎水効果を得るために、ホットプレートで30分間加熱し、引張り可能な可撓超疎液性フィルムが得られた。
<実施例2>
The present embodiment provides a method for producing a pullable flexible ultra-phobic film and includes the following steps.
(1) The original template having a T-type micro / nano structure was washed and dried, and then placed on a hot plate. The temperature of the hot plate was set to 150 ° C. A clean glass slide was placed next to the template and preheated for 3 minutes. Perfluorodecyltrichlorosilane (PFTS) was removed, 2 drops were dropped on a slide on a hot plate using a disposable pipette, and the surface of the original template on the hot plate was covered with a glass dish. In order to obtain the highest hydrophobic effect, it was heated on a hot plate for 4 minutes.
(2) Remove the covered glass dish, pour polydimethylsiloxane (PDMS), a curable elastic material prepared in advance, into a culture dish, place in a vacuum dryer at 80 ° C., and bake in a vacuum atmosphere for 2 hours to cure The elastic elastic material PDMS was cured. After peeling off the curable elastic material PDMS, an intermediate having a T-type micro / nano structure on the surface was obtained.
(3) A PDMS intermediate having a T-type micro / nano structure on the surface is set on a spin coater so that the microstructure surface faces up, and a liquid EVA emulsion is flowed into the surface of the intermediate, and the rotational speed is 50 rpm to In the range of 2000 rpm, different spin coating speeds can be set according to the desired thickness. For example, at 100 rpm, the thickness is about 160 μm, and at 300 rpm, the thickness is about 80 μm.
(4) The EVA emulsion after spin coating was taken out together with the PDMS intermediate, and cured in a low temperature atmosphere of −4 ° C. or lower. Curing time increases with EVA emulsion thickness. After curing, the film was peeled from the PDMS intermediate having a T-type micro / nano structure, and an EVA film having a T-type micro / nano structure on the surface was obtained.
(5) An EVA film having a T-type micro / nano structure was set on a hot plate so that both ends were supported and suspended. The temperature of the hot plate was set to 70 ° C. A clean glass slide was placed next to the film and preheated for 3 minutes. Several drops of perfluorodecyltrichlorosilane (PFTS) were dropped on a slide glass on a hot plate using a disposable pipette, and the hot plate was covered from above with a glass dish. In order to obtain the highest hydrophobic effect, the film was heated on a hot plate for 30 minutes to obtain a flexible ultra-liquidphobic film that can be pulled.
<Example 2>
本実施例は液滴の非破壊性移動方法を提供する。図2に示される過程のように、本実施例において、実施例1で作製された超疎液性表面の良好な柔軟性と良好な引張り性とを有する特徴を利用して液滴操作及び非破壊性移動を行うことができる。具体的には、該方法は、以下のステップを含む。
まず、液滴22を超疎液性フィルム23に置くこと。
つぎに、実施例1で作製された可撓透明超疎液性フィルム21を操作し、超疎液性フィルム23から液滴を捕獲すること。
最後に、超疎液性フィルム21を引っ張ってフィルムの液滴に対する粘着力を低減させ、液滴22をフィルムから落下させ、非破壊的に他の任意の表面に移動させること。
<実施例3>
This example provides a non-destructive transfer method for droplets. As in the process shown in FIG. 2, in this example, droplet operation and non-utilization are performed using the characteristics of the super lyophobic surface produced in Example 1 having good flexibility and good tensile properties. Destructive transfer can be performed. Specifically, the method includes the following steps.
First, the
Next, the flexible transparent super
Finally, pulling the super
<Example 3>
本実施例は他の液滴の非破壊性移送方法を提供する。本実施例において、実施例1で作製された超疎液性表面の良好な柔軟性と良好な引張り性とを有する特徴を利用して液滴操作及び非破壊性移動を行うことができる。具体的には、該方法は、以下のステップを含む。
まず、液滴22を超疎液性フィルム23に置くこと。
つぎに、実施例1で作製された可撓透明超疎液性フィルム21を操作し、超疎液性フィルム23から液滴を捕獲すること。
最後に、超疎液性フィルム21を湾曲させることにより、フィルムと液滴との接触部の局所の曲率を変化させ、フィルムの液滴に対する粘着力を低減させ、液滴22をフィルムから落下させ、非破壊的に他の任意の表面に移動させること。
This embodiment provides another non-destructive transfer method for droplets. In this example, droplet manipulation and non-destructive transfer can be performed using the characteristics of the super-lyophobic surface produced in Example 1 having good flexibility and good tensile properties. Specifically, the method includes the following steps.
First, the
Next, the flexible transparent super
Finally, by curving the super
図3は、本発明にかかる引張り可能な可撓超疎液性表面によって実際に液滴を操作し、液滴の非破壊性移動を実現する操作過程を示す図である。図3から、本発明により提供される技術を採用することによって、液滴の非破壊性伝送を効果的に実現できることが分かる。 FIG. 3 is a diagram showing an operation process in which a droplet is actually manipulated by the pullable flexible super-lyophobic surface according to the present invention to realize non-destructive movement of the droplet. FIG. 3 shows that non-destructive transmission of droplets can be effectively realized by employing the technique provided by the present invention.
Claims (12)
(2)硬化した後に、前記硬化性弾性材料をオリジナルテンプレートから剥離し、前記オーバーハングマイクロ・ナノ構造に対応するマイクロ・ナノ構造を有する中間体を得るステップ、
(3)前記中間体の前記オーバーハングマイクロ・ナノ構造に対応するマイクロ・ナノ構造を有する層の表面にプラスチックエマルジョンをスピンコートするステップ、
(4)スピンコートされたプラスチックエマルジョンを硬化させ、フィルムを形成するステップ、及び
(5)硬化した前記フィルムを剥離し、フッ素化修飾を行い、引張り可能な可撓超疎液性フィルムを得るステップ、
を含み、
前記ステップ(3)において、前記プラスチックエマルジョンが、EVAエマルジョンである、
引張り可能な可撓超疎液性フィルムの製造方法。 (1) performs a fluorinated modifications to template having an overhang micro-nano structures, Komu to flow the curable elastomeric material step,
(2) after curing, peeling the curable elastic material from the original template to obtain an intermediate having a micro-nano structure corresponding to the overhanging micro-nano structure;
(3) spin-coating a plastic emulsion on the surface of the layer having a micro-nanostructure corresponding to the overhanging micro-nanostructure of the intermediate;
(4) curing the spin-coated plastic emulsion, forming a film, and (5) was peeled off the cured the film was, had row fluorinated modification, the pull tension capable flexible super hydrophobic film Getting step,
Only including,
In the step (3), the plastic emulsion is an EVA emulsion.
A method for producing a pullable flexible ultra-liquidphobic film.
前記オリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面を化学気相蒸着プロセスによって加熱処理して、プラズマ状態のフッ化炭素化合物ガス源でオーバーハングマイクロ・ナノ構造の各々の方向に蒸着を行い、前記オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップ、或いは
単分子自己組織化プロセスによって前記オリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面において化学反応を起こさせ、前記オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップを含む、
請求項1に記載の製造方法。 In step (1), the fluorination modification comprises
The surface of the overhanging micro / nanostructure of the original template is heat-treated by a chemical vapor deposition process, and vapor deposition is performed in each direction of the overhanging micro / nanostructure with a fluorocarbon compound gas source in a plasma state. Generating a hydrophobic fluorocarbon compound coating on the surface of the overhanging micro / nanostructure, or causing a chemical reaction on the surface of the overhanging micro / nanostructure of the original template by a single molecule self-assembly process, including the step of generating a hydrophobic fluorocarbon compound coated on the surface of the overhang micro and nano structures,
The manufacturing method according to claim 1.
前記オリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面を化学気相蒸着プロセスによって加熱処理して、プラズマ状態のフッ化炭素化合物ガス源でオーバーハングマイクロ・ナノ構造の各々の方向に蒸着を行い、前記オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップ、或いは
単分子自己組織化プロセスによって前記オリジナルテンプレートのオーバーハングマイクロ・ナノ構造の表面において化学反応を起こさせ、前記オーバーハングマイクロ・ナノ構造の表面に疎水性のフッ化炭素化合物コーティングを生成するステップを含む、
請求項1に記載の製造方法。 In step (5), the fluorination modification comprises
The surface of the overhanging micro / nanostructure of the original template is heat-treated by a chemical vapor deposition process, and vapor deposition is performed in each direction of the overhanging micro / nanostructure with a fluorocarbon compound gas source in a plasma state. Generating a hydrophobic fluorocarbon compound coating on the surface of the overhanging micro / nanostructure, or causing a chemical reaction on the surface of the overhanging micro / nanostructure of the original template by a single molecule self-assembly process, including the step of generating a hydrophobic fluorocarbon compound coated on the surface of the overhang micro and nano structures,
The manufacturing method according to claim 1.
もう一枚の請求項1−8のいずれか1項に記載の引張り可能な可撓超疎液性フィルムの製造方法により得られた引張り可能な可撓超疎液性フィルムの表面を前記液滴に接触させることで、前記液滴を捕獲して移動させるステップ2、及び
マイクロ・ナノ構造のピッチを増加させ、固液接触面積を減らして、前記液滴を前記引張り可能な可撓超疎液性フィルムの表面から落下させ、移動を終了するステップ3を含む、
液滴の非破壊性移動方法。 Step 1 of placing the droplet on the surface of any one can pull according to a flexible super hydrophobic possible flexible super hydrophobic film tension obtained by the film production method of claim 1 8,
The surface of the pullable flexible super lyophobic film obtained by the method for producing a pullable flexible super lyophobic film according to any one of claims 1 to 8 is used as the droplet. Step 2 of capturing and moving the droplet by bringing it into contact, and increasing the pitch of the micro-nano structure, reducing the solid-liquid contact area, and allowing the droplet to be pulled and the flexible ultra-lyophobic liquid is dropped from the surface of the sex film, including a step 3 to end the movement,
Non-destructive transfer method of droplets.
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CN113578406A (en) * | 2021-09-07 | 2021-11-02 | 北京航空航天大学 | Microcolumn surface for droplet transfer, method for producing microcolumn surface, and droplet transfer method |
CN113830727B (en) * | 2021-09-09 | 2024-05-24 | 中国人民解放军军事科学院国防科技创新研究院 | Transfer method of micro-nano piece |
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