WO2003076038A1 - Procede d'enrichissement d'une phase liquide a l'interieur d'une micropuce par ecoulement diphase gaz-liquide et dispositif a micropuces associe - Google Patents

Procede d'enrichissement d'une phase liquide a l'interieur d'une micropuce par ecoulement diphase gaz-liquide et dispositif a micropuces associe Download PDF

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Publication number
WO2003076038A1
WO2003076038A1 PCT/JP2003/002337 JP0302337W WO03076038A1 WO 2003076038 A1 WO2003076038 A1 WO 2003076038A1 JP 0302337 W JP0302337 W JP 0302337W WO 03076038 A1 WO03076038 A1 WO 03076038A1
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WO
WIPO (PCT)
Prior art keywords
gas
liquid
phase
flow
microchip
Prior art date
Application number
PCT/JP2003/002337
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English (en)
Japanese (ja)
Inventor
Takehiko Kitamori
Manabu Tokeshi
Akihide Hibara
Original Assignee
Kanagawa Academy Of Science And Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Kanagawa Academy Of Science And Technology filed Critical Kanagawa Academy Of Science And Technology
Priority to JP2003574302A priority Critical patent/JP4424993B2/ja
Publication of WO2003076038A1 publication Critical patent/WO2003076038A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0031—Degasification of liquids by filtration

Definitions

  • the invention of this application relates to a method for concentration in a microchip by a gas-liquid two-phase flow and a microchip device therefor.
  • the invention of this application has an object to integrate a concentration method involving a volume change as an operation on a microchip, based on the development of a microchemical system by the inventors and their knowledge so far.
  • a liquid-phase two-phase flow is formed in the flow path to form a liquid-phase interface.
  • a method for concentrating in a microphone-mouth chip by gas-liquid two-phase flow which is characterized by performing concentration.
  • the invention of this application is characterized in that the above-mentioned enrichment method is characterized in that the flow rate ratio between the gas phase and the liquid phase in the flow path is controlled so that gas phase> liquid phase.
  • the fourth is a condensing method characterized by forming a gas-liquid interface in multiple stages by introducing gas into the flow path in multiple stages and discharging the gas. Fourth, a gas-liquid two-phase flow is used.
  • a concentration method characterized by heating at least a part of a formed flow path to evaporate a part of a liquid phase solvent.
  • the invention of this application is a device for concentrating a liquid phase by forming an interface by a gas-liquid two-phase flow in a flow channel in a microchip having a flow channel formed in a substrate.
  • a microchip device in which a gas and a liquid constituting a gas-liquid two-phase flow are respectively provided with an introduction path and a discharge path.
  • the above-mentioned microchip device is characterized in that a flow rate control mechanism for controlling the flow rate ratio in the flow path to be gas phase> liquid phase is provided.
  • a flow rate control mechanism for controlling the flow rate ratio in the flow path to be gas phase> liquid phase is provided.
  • On the bottom of the flow channel there is provided a ridge in the flow direction corresponding to the position of the gas-liquid interface, and the arrangement of the ridge is at least part of the flow control mechanism.
  • a micro flow path is provided in which a gas is introduced into the flow path in multiple stages to form a gas-liquid interface in the flow path in multiple stages, and the gas is discharged in accordance with the multi-stage flow.
  • the ninth is a microchip device characterized in that a heating mechanism for heating at least a part of a flow path in which a gas-liquid two-phase flow is formed is provided. In the case of 0, heat is applied to the back of the substrate on which the flow path is provided or to the surface of the upper plate.
  • the present invention
  • FIG. 1 is a schematic diagram showing the basic configuration of the invention of this application.
  • FIG. 2 is a cross-sectional view showing an example of an asymmetric microchannel having a ridge.
  • FIG. 3 is a schematic process diagram illustrating a method for forming a fine channel having a ridge.
  • FIG. 4 is a schematic process diagram illustrating a two-step etching method for forming an asymmetric fine channel.
  • Fig. 5 is a schematic diagram illustrating the arrangement of the Hi-Ichi Line.
  • FIG. 6 is a schematic process diagram illustrating a method for forming a line of heaters.
  • FIG. 7 is a schematic cross-sectional view of an asymmetric fine channel as an example.
  • FIG. 8 is a schematic perspective view of a microchip as an embodiment provided with a microheater.
  • FIG. 9 is a diagram illustrating the relationship between the concentration and the applied voltage in the example.
  • ⁇ FIG. 10 is a schematic diagram of a three-stage channel.
  • FIG. 11 is a diagram exemplifying a stable condition of a two-phase flow of ethyl acetate and air.
  • FIG. 12 is a diagram illustrating a stable condition of a two-phase flow of water and air.
  • symbol in a figure shows the following.
  • an interface is formed by a gas-liquid two-phase flow of gas and liquid in a fine channel (microchannel) formed on a substrate of a microchip to concentrate the liquid phase. It is fundamental to do.
  • This enrichment method is an enrichment operation in a small, limited space called a microchannel, which has a large specific interfacial area, a high evaporation rate of the solvent, and is performed under the restriction of gas-liquid equilibrium. It has a fundamental feature that control is easy because it is maintained.
  • FIG. 1 is a schematic diagram showing the basics of the enrichment method of the invention of this application.
  • a microchannel (2) formed by microfabrication such as etching is provided on a microchip substrate (1) made of glass, ceramics, silicon, resin, or the like.
  • a gas-liquid two-phase flow of a gas phase (3A) and a liquid phase (3B) is formed, and a solvent constituting the liquid phase (3B) is formed at the interface (3C). It is evaporated and concentrated.
  • the cover upper plate is placed in close contact to prevent the gas phase (3A) from dissipating the liquid phase (3B).
  • the gas introduction path (4 A) and the liquid introduction path (4 B) for forming the gas-liquid two-phase flow, and the gas discharge path (5A) and the liquid discharge path (5 B) are the same. It is arranged on the substrate (1) by fine processing.
  • the size and length of the microchannel (2) are not particularly limited, but are appropriately set for configuring a microchemical system on a microchip.
  • a practical guideline is that the width is 500 / xm or less and the depth is about 300 im or less.
  • the fine channel Since it is necessary to form an interface due to gas-liquid two-phase flow in the channel, the cross-sectional area of the microchannel and the types of substances constituting each of the gas phase and the liquid phase are taken into consideration. A suitable gas-phase and liquid-phase flow ratio for interface formation will be set.
  • the flow rate ratio between the gas phase (3A) and the liquid phase (3B) in the microchannel (2) is set so that the flow rate of the gas phase is larger than the flow rate of the liquid phase. It is desirable to control. However, if the flow rate of the gas phase is excessive or excessive with respect to the flow rate of the liquid phase, liquid phase substances are mixed in the gas phase, and an interface as a gas-liquid two-phase flow is not formed. Of course, conversely, even when the gas flow rate is too small, the formation of the interface becomes difficult.
  • the flow rate ratio between the gas phase and the liquid phase is gas phase> liquid phase.
  • the microchip is provided with a mechanism as an auxiliary means for controlling the flow ratio with high accuracy.
  • a ridge (6) in the flow direction corresponding to the position of the gas-liquid interface is provided at the bottom of the microchannel (2), as shown in the cross-section in Fig. 2. It is considered that the flow rate ratio between the gas phase (3A) and the liquid phase (3B) can be controlled by selecting the location of the ridge (6).
  • the ridge (6) plays the role of a guide, and not only when it is strictly located at the gas-liquid interface (3C), but also a gas-liquid two-phase flow and a predetermined flow rate ratio are ensured. It goes without saying that, under the condition, there may be a deviation from the gas-liquid interface (3 C) position at an allowable position as shown in FIG.
  • a microchannel (2) having an asymmetrical cross section is one of the effective means for increasing the gas flow rate.
  • a photoresist is disposed on a metal deposition film on the surface of a glass substrate, and UV light is irradiated through a mask. Transfer and then metal etching ⁇ hydrofluoric acid etching and development ⁇ photolithography and etching
  • FIG. 5 shows an example in which such a heater line (7) is provided.
  • FIG. 6 it can be easily formed by etching a Cr vapor deposition film.
  • a plurality of interfaces by gas-liquid two-phase flow as described above may be provided intermittently so that concentration operation can be performed in multiple stages.
  • it is considered to provide multiple gas flow paths for introducing and discharging the gas at each stage.
  • the invention of the present application as described above enables highly efficient concentration operation on a microchip.
  • a Co-DMAP complex in ethyl acetate was introduced from one of the double Y-type microchannels, and air was introduced from the other inlet to create a gas-liquid two-layer structure in the microchannel.
  • a flow is formed, and the organic phase is measured along a microchannel with a thermal lens microscope, and concentrated as a change in the concentration of Co-DMAP complex per unit volume based on the relationship between the measurement position of the thermal lens microscope and the signal intensity. The efficiency was evaluated. And increase the concentration efficiency from the viewpoint of vapor-liquid equilibrium.
  • a chip with asymmetric microchannel cross section (Fig. 7) was used.
  • a micro-hidden was prepared on the back of the microchip and concentrated by heating.
  • an asymmetric microchannel having the cross section shown in FIG. 7 was prepared by using the two-step etching method illustrated in FIG. 4, and the flow rate ratio was set to 1: 200 using this channel to perform measurement. In this case, a concentration of about 2 times was obtained, and evaporation in the microchip was confirmed. Furthermore, in order to increase the concentration efficiency, a micro-heater was fabricated by patterning a Cr thin film on the back surface of the microchip by etching as shown in Fig. 6 (Fig. 8), and the chip was locally heated. Fig. 9 shows the results of concentration measurement at a point of 30 mm after two-phase merging using this chip.
  • the heat lens signal intensity increases with an increase in applied voltage, that is, a rise in temperature, indicating that the enrichment is improved by heating. From the signal intensity, the enrichment was more than 4 times (75% of the solvent evaporated) by volume change.
  • Fig. 11 shows the case of air and ethyl acetate
  • Fig. 12 shows the case of air and water
  • region A in the figure shows the stable condition
  • region B shows the unstable condition due to excess air.
  • the C region indicates that the liquid is excessive and unstable.
  • the enrichment method can be integrated on a microchip, and highly efficient enrichment can be achieved. This is very useful for the detection, measurement, and separation / recovery of environmentally regulated substances in the liquid phase, biologically related substances, biological substances, and trace substances such as reaction intermediates and reagents. Concentration on a microchip becomes possible.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Micromachines (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

L'invention concerne un procédé permettant d'enrichir une phase liquide à l'intérieur d'une micropuce ayant un passage d'écoulement formé dans son substrat, qui consiste à former une face limite dans ledit passage par un écoulement diphasé gaz-liquide destiné à enrichir la phase liquide, le procédé d'enrichissement, suivi d'un changement volumétrique, étant intégré dans la micropuce et la phase liquide pouvant être enrichie de manière très efficace.
PCT/JP2003/002337 2002-03-14 2003-02-28 Procede d'enrichissement d'une phase liquide a l'interieur d'une micropuce par ecoulement diphase gaz-liquide et dispositif a micropuces associe WO2003076038A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2003574302A JP4424993B2 (ja) 2002-03-14 2003-02-28 気液二相流でのマイクロチップ内濃縮方法とそのためのマイクロチップデバイス

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2002070986 2002-03-14
JP2002-070986 2002-03-14

Publications (1)

Publication Number Publication Date
WO2003076038A1 true WO2003076038A1 (fr) 2003-09-18

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JP (1) JP4424993B2 (fr)
WO (1) WO2003076038A1 (fr)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005169386A (ja) * 2003-11-17 2005-06-30 Kanagawa Acad Of Sci & Technol マイクロチャンネル内表面の部分化学修飾方法とマイクロチャンネル構造体
JP2005285577A (ja) * 2004-03-30 2005-10-13 Casio Comput Co Ltd 気化装置、反応装置及び発電装置
JP2007260858A (ja) * 2006-03-29 2007-10-11 Sumitomo Bakelite Co Ltd プラスチックへのマイクロ流路形成方法、及びその方法を利用して製造されたプラスチック製バイオチップもしくはマイクロ分析チップ
WO2009057693A1 (fr) 2007-11-01 2009-05-07 Jfe Engineering Corporation Micropuce, dispositif à micropuces et procédé d'opération d'évaporation utilisant la micropuce

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997047390A1 (fr) * 1996-06-14 1997-12-18 University Of Washington Appareil d'extraction differentielle a absorption amelioree
JP2001137613A (ja) * 1999-11-11 2001-05-22 Kawamura Inst Of Chem Res 抽出機構を有する微小ケミカルデバイス

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997047390A1 (fr) * 1996-06-14 1997-12-18 University Of Washington Appareil d'extraction differentielle a absorption amelioree
JP2001137613A (ja) * 1999-11-11 2001-05-22 Kawamura Inst Of Chem Res 抽出機構を有する微小ケミカルデバイス

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005169386A (ja) * 2003-11-17 2005-06-30 Kanagawa Acad Of Sci & Technol マイクロチャンネル内表面の部分化学修飾方法とマイクロチャンネル構造体
JP4523386B2 (ja) * 2003-11-17 2010-08-11 財団法人神奈川科学技術アカデミー マイクロチャンネル内表面の部分化学修飾方法とマイクロチャンネル構造体
JP2005285577A (ja) * 2004-03-30 2005-10-13 Casio Comput Co Ltd 気化装置、反応装置及び発電装置
JP2007260858A (ja) * 2006-03-29 2007-10-11 Sumitomo Bakelite Co Ltd プラスチックへのマイクロ流路形成方法、及びその方法を利用して製造されたプラスチック製バイオチップもしくはマイクロ分析チップ
WO2009057693A1 (fr) 2007-11-01 2009-05-07 Jfe Engineering Corporation Micropuce, dispositif à micropuces et procédé d'opération d'évaporation utilisant la micropuce
JP2009106916A (ja) * 2007-11-01 2009-05-21 Jfe Engineering Corp マイクロチップ、マイクロチップデバイス及びマイクロチップを用いた蒸発操作方法
US9120032B2 (en) 2007-11-01 2015-09-01 Jfe Engineering Corporation Microchip, microchip device, and evaporation operation method using the microchip

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JP4424993B2 (ja) 2010-03-03
JPWO2003076038A1 (ja) 2005-06-30

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