The present invention relates to a flow cell which can be used as a flowmeter or an electric conductivity meter for use in an analytical instrument, a fluorescence detector for liquid chromatography, a microchip for electrophoretic separation, or the like and a method for producing such a flow cell.
In recent years, various flow cells capable of handling a trace amount of fluid have been developed using semiconductor manufacturing techniques such as etching used to form a fine groove or the like.
This flow cell includes a plate-shaped member 34 having a groove as a flow path 7 formed in the surface thereof and a plate-shaped member 32 having through holes 9 and 11 formed at positions corresponding to both ends of the groove, and it is obtained by bonding together the plate-shaped member 32 and the plate-shaped member 34.
Examples of the plate-shaped members 32 and 34 conventionally used include glass substrates, silicon substrates, and resin substrates. For example, in a case where a glass substrate or a silicon substrate is used as the plate-shaped member 34, a groove can be formed by etching using a chemical solution or a reactive gas. On the other hand, in a case where a resin substrate is used as the plate-shaped member 34, a groove can be formed by molding.
A method for bonding together the plate-shaped members 32 and 34 depends on the materials thereof. For example, in a case where the plate-shaped members 32 and 34 are both silicon substrates, a diffusion bonding method is typically used. Further, in a case where the plate-shaped members 32 and 34 are both glass substrates or resin substrates, a heat sealing method is typically used. Furthermore, in a case where one of the plate-shaped members 32 and 34 is a silicon substrate and the other is a glass substrate, an anodic bonding method is typically used.
Even such a conventional flow cell can handle a trace amount of fluid. However, in a case where a silicon substrate or a glass substrate is used as a plate-shaped member to produce such a conventional flow cell, it is necessary to form a groove using semiconductor manufacturing techniques such as etching using a chemical solution or a reactive gas. This requires an exposure device for transferring the shape of a groove onto the plate-shaped member, facilities for a chemical solution or a reactive gas to be used, and the like, thereby resulting in high production costs.
On the other hand, in a case where a resin substrate is used as a plate-shaped member to produce such a conventional flow cell, there is an advantage that a groove can be formed by molding and therefore the cost for forming a groove can be reduced. However, resin is poor in resistance to organic solvents, and therefore, such a conventional flow cell has limited uses.
In order to eliminate the necessity to form a groove in a glass substrate by etching for cost reduction and to improve resistance to organic solvents, Japanese Patent Application Laid-open No. H8-35927 (hereinafter, simply referred to as “Patent Document 1”) proposes a flow cell using a glass substrate having a groove formed therein as a plate-shaped member. This flow cell is obtained by interposing a fluorocarbon resin as a spacer between two glass substrates to obtain a laminate, holding both ends of the laminate, and applying pressure to both ends of the laminate to bring the fluorocarbon resin into close contact with the glass substrates.
However, when the spacer is interposed between the glass substrates and only pressure is applied, with no bonding, a gap is formed between each glass substrate and the spacer. Particularly, pressure is not applied to the central area of the flow cell, and therefore liquid leakage is likely to occur at the central area of the flow cell. Particularly, liquid leakage is likely to occur when an organic solvent flows through the flow cell.
It is therefore an object of the present invention to provide a flow cell which can be produced at lower cost without forming a groove in a plate-shaped member by etching and which is free from liquid leakage and excellent in chemical resistance.
In order to achieve the above object, the present invention is directed to a flow cell including: a flow path member, at least a surface layer of which is made of a fluorocarbon resin, the surface layer having a groove as a flow path formed therein; and a cover member bonded to the surface layer of the flow path member by the fluorocarbon resin itself, wherein at least either the flow path member or the cover member has two through holes as a fluid inlet and a fluid outlet formed at positions corresponding to both ends of the groove.
The flow path member according to one embodiment of the present invention has a structure in which a fluorocarbon resin film is laminated on the surface of a flat plate-shaped member, and therefore the fluorocarbon resin film serves as the surface layer made of a fluorocarbon resin. In this case, the groove is constituted from a through hole formed in the fluorocarbon resin film and the surface of the flat plate-shaped member. Further, the fluorocarbon resin film itself interposed between the flat plate-shaped member and the cover member bonds these members together.
The flow path member according to another embodiment of the present invention is formed from a fluorocarbon resin body entirely made of a fluorocarbon resin, and therefore, a surface layer of the fluorocarbon resin body serves as the surface layer made of a fluorocarbon resin. In this case, the groove is a recess formed in the surface of the fluorocarbon resin body.
Further, the fluorocarbon resin film or the fluorocarbon resin body can be made of an adhesive fluorocarbon resin which exhibits adhesiveness to a substrate made of another material at a certain temperature or higher.
The adhesive fluorocarbon resin exhibits adhesiveness also to a substrate made of another material, such as a glass substrate, a metal plate, or a silicon substrate, at a certain temperature (e.g., at a temperature near its glass transition temperature). However, at a temperature lower than the certain temperature, the surface of the adhesive fluorocarbon resin exhibits self-adsorption properties only. Therefore, bonding between the flow path member and the cover member is carried out at a temperature near or higher than the glass transition temperature of the adhesive fluorocarbon resin but lower than the decomposition temperature of the adhesive fluorocarbon resin. In order to further improve adhesion between the flow path member and the cover member, bonding between the flow path member and the cover member is preferably carried out at a temperature near or higher than the melting point of the adhesive fluorocarbon resin but lower than the decomposition temperature of the adhesive fluorocarbon resin. As such an adhesive fluorocarbon resin, Neoflon™ EFEP (manufactured by Daikin Industries, Ltd.) or the like can be used.
Further, at least a part of the bonding surface between the flow path member and the cover member is preferably covered with a metal layer. Further, the metal layer preferably covers the glass substrate including the edge of the groove, or the ‘flow path’.
The present invention is also directed to a method for producing a flow cell, including the steps of:
(A) forming a through hole in the form of a groove as a flow path in a fluorocarbon resin film;
(B) forming two through holes as a liquid inlet and a liquid outlet in either a flat plate-shaped member or a cover member at positions corresponding to both ends of the groove; and
(C) interposing the fluorocarbon resin film between the flat plate-shaped member and the cover member so that one end of the groove is aligned with one of the through holes and the other end of the groove is aligned with the other through hole to obtain a laminate, and heating and pressing the laminate until the fluorocarbon resin film exhibits adhesiveness so that the fluorocarbon resin film bonds the flat plate-shaped member and the cover member together.
The present invention is also directed to another method for producing a flow cell, including the steps of:
(A) laminating a fluorocarbon resin body on the surface of a molding die having a projection formed thereon by which a groove as a flow path is to be formed, and relatively pressing the fluorocarbon resin body against the molding die to mold the fluorocarbon resin body while heating the fluorocarbon resin body to a temperature near the melting point of the fluorocarbon resin body;
(B) forming two through holes as a liquid inlet and a liquid outlet in the fluorocarbon resin body or a cover member at positions corresponding to both ends of the groove; and
(C) laminating the cover member on the molded surface of the fluorocarbon resin body (in a case where the through holes are formed in the cover member, the cover member is laminated on the molded surface of the fluorocarbon resin body so that one end of the groove is aligned with one of the through holes as a liquid inlet and the other end of the groove is aligned with the other through hole as a liquid outlet) and pressing the laminate while heating until the fluorocarbon resin body exhibits adhesiveness to bond the fluorocarbon resin body and the cover member together.
The temperature to which the fluorocarbon resin film or the fluorocarbon resin body is heated to allow the fluorocarbon resin film or the fluorocarbon resin body to exhibit adhesiveness can be set to a temperature equal to or higher than the melting point of a fluorocarbon resin constituting the fluorocarbon resin film or the fluorocarbon resin body but lower than the decomposition temperature of the fluorocarbon resin.
As the fluorocarbon resin, an adhesive fluorocarbon resin can be used. In this case, the temperature to which the fluorocarbon resin film or the fluorocarbon resin body is heated to allow the fluorocarbon resin film or the fluorocarbon resin body to exhibit adhesiveness can be set to a temperature equal to or higher than the temperature, at which the adhesive fluorocarbon resin begins to exhibit adhesiveness, but lower than the decomposition temperature of the adhesive fluorocarbon resin.
The method for producing a flow cell according to the present invention may further include, prior to bonding the flow path member and the cover member together, the step of forming a metal layer on at least a part of the surface of either of the members to be bonded to the fluorocarbon resin film or the fluorocarbon resin body.
As described above, in the case of the conventional flow cell disclosed in Patent Document 1, there is a case where a gap is formed between members constituting the flow cell only by holding both ends of the flow cell and applying pressure to both ends of the flow cell, and therefore a solvent or the like leaks from the gap. On the other hand, in the case of the flow cell according to the present invention, the flow cell is heated and pressed to allow a fluorocarbon resin interposed between members constituting the flow cell to bond these members together, thereby increasing the bonding strength between these members and therefore preventing formation of a gap and leakage of a solvent.
As described above, since the fluorocarbon resin itself bonds members constituting the flow cell together, liquid leakage is less likely to occur in the flow cell according to the present invention than in a flow cell obtained by pressing a laminate of two substrates, between which a spacer is interposed, to bring these substrates into close contact with each other. Therefore, it is not necessary for the flow cell according to the present invention to use a jig for applying pressure to substrates to keep close contact between these substrates, thereby reducing the size of the flow cell. Further, in the case of the conventional flow cell disclosed in Patent Document 1, both ends of the flow cell are pressed using screws, which makes it difficult to stack the flow cells to produce a multiple flow cell having multiple flow paths. In addition, in order to change some of the flow cells of such a multiple flow cell, it is necessary to completely disassemble the multiple flow cell. On the other hand, in the case of a multiple flow cell using the flow cells according to the present invention, the flow cells are independent of one another, and therefore some of the flow cells can be easily changed.
Further, since the flow path of the flow cell according to the present invention is formed in the fluorocarbon resin, the flow cell according to the present invention can handle organic solvents and the like which cannot be handled by conventional flow cells made of acrylic resin or polycarbonate resin.
By using an adhesive fluorocarbon resin as the fluorocarbon resin, a groove can be more easily formed in the adhesive fluorocarbon resin by molding or cutting. Therefore, it is possible to form a groove as a flow path at lower cost as compared to a case where a groove is formed in a glass substrate or a silicon substrate.
Further, by forming a metal thin film on the surface of a member to be bonded to the fluorocarbon resin, it is possible to enhance bonding strength between members constituting the flow cell according to the present invention, thereby improving the reliability of the flow cell according to the present invention. Further, by using the metal thin film as electrodes, it is also possible to allow the flow cell according to the present invention to have higher performance.
Hereinbelow, preferred embodiments of the present invention will be described with reference to the accompanying drawings. It is to be noted that these preferred embodiments use an adhesive fluorocarbon resin as a fluorocarbon resin, but a fluorocarbon resin other than the adhesive fluorocarbon resin can also be used in the present invention.
The flow cell according to the first embodiment includes a plate-shaped glass substrate 3, an adhesive fluorocarbon resin sheet 5 having a groove as a flow path 7 formed by cutting, and a glass substrate 1 as a cover member having through holes 9 and 11 as a fluid inlet and a fluid outlet formed at positions corresponding to both ends of the groove. The fluorocarbon resin sheet 5 is interposed between the glass substrates 1 and 3, and the fluorocarbon resin sheet 5 itself bonds the glass substrate 1 and the glass substrate 3 together. The glass substrate 3 and the fluorocarbon resin sheet 5 bonded to the glass substrate 3 constitute a flow path member 17.
The fluorocarbon resin sheet 5 is formed using Neoflon™ EFEP RP-4020, and therefore has a melting point of 155 to 170° C. and a decomposition temperature of 355° C.
Each of the glass substrates 1 and 3 has flat surfaces. In the glass substrate 1, through holes 9 and 11 as a fluid inlet and a fluid outlet are formed by, for example, ultrasonic machining or sandblasting.
In the fluorocarbon resin sheet 5, a through groove as a flow path 7 is formed between positions corresponding to the through holes 9 and 11 formed in the glass substrate 1, and the through groove is formed by, for example, cutting using a cutting plotter. It is to be noted that as shown in
Then, the fluorocarbon resin sheet 5 having a through groove formed by cutting is laminated on the glass substrate 3 having flat surfaces, and then the glass substrate 1 is further laminated on the fluorocarbon resin sheet 5 so that one end of the flow path 7 of the fluorocarbon resin sheet 5 is aligned with the through hole 9 and the other end of the flow path 7 is aligned with the through hole 11. The obtained laminate is pressed at a pressure of about 10 kPa while heated to 250° C., which is higher than the melting point of the fluorocarbon resin sheet 5 but lower than the decomposition temperature of the fluorocarbon resin sheet 5, to allow the fluorocarbon resin sheet 5 to bond the glass substrate 1 and the glass substrate 3 together, and is then cooled to obtain a flow cell.
The fluorocarbon resin sheet 5 can also be formed using Neoflon™ EFEP RP-5000. However, Neoflon™ EFEP RP-5000 has a melting point of 190 to 200° C. and a decomposition temperature of 380° C., and therefore, in a case where the fluorocarbon resin sheet 5 is formed using Neoflon™ EFEP RP-5000, it is necessary to carry out bonding between the glass substrates 1 and 3 at a higher temperature as compared to the above-described case where the fluorocarbon resin sheet 5 is formed using Neoflon™ EFEP RP-4020.
Hereinbelow, a flow cell according to another embodiment (a second embodiment) of the present invention will be described with reference to
The flow cell according to the second embodiment includes: a fluorocarbon resin body 27 entirely made of an adhesive fluorocarbon resin and having a groove as a flow path 7 formed in the surface thereof; and a glass substrate 1 as a cover member provided to cover the groove of the fluorocarbon resin body 27. The flow cell according to the second embodiment is obtained by bonding the fluorocarbon resin body 27 and the glass substrate 1 together by means of adhesiveness of the adhesive fluorocarbon resin. The glass substrate 1 has through holes 9 and 11 formed at positions corresponding to both ends of the groove as a flow path 7, and the through holes 9 and 11 will function as a fluid inlet 9 for introducing a fluid into the flow path 7 and a fluid outlet 11 for discharging the fluid from the flow path 7.
The fluorocarbon resin body 27 is formed using, for example, Neoflon™ EFEP RP-4020 which is also used in the first embodiment.
Hereinbelow, a method for producing a flow cell according to the second embodiment will be described with reference to
(A) A silicon substrate 21, which is a mold for forming a groove in the fluorocarbon resin body 27, has a structure (a projection 23) formed by, for example, photoengraving and etching using an alkaline chemical solution.
The adhesive fluorocarbon resin body 27 is laminated on the surface of the silicon substrate 21 having the projection 23 formed thereon, and the laminate is heated to, for example, 150° C. and pressed at, for example, 0.4 MPa to form a groove as a flow path 7 in the surface of the fluorocarbon resin body 27. The temperature for heating the laminate is preferably near the melting point of the adhesive fluorocarbon resin.
(B) As in the case of the first embodiment, through holes 9 and 11 as a fluid inlet and a fluid outlet are formed in a flat plate-shaped glass substrate 1 as a cover member by, for example, ultrasonic machining or sandblasting.
(C) The glass substrate 1 is laminated on the fluorocarbon resin body 27 having a groove formed therein so that one end of the flow path 7 is aligned with the through hole 9 and the other end of the flow path 7 is aligned with the through hole 11, and the obtained laminate is heated to 250° C. and pressed at about 10 kPa to bond the glass substrate 1 and the fluorocarbon resin body 27 together to obtain a flow cell.
Hereinbelow, a flow cell according to yet another embodiment (a third embodiment) of the present invention will be described.
As described above, the flow cell according to the first embodiment or the second embodiment is obtained by laminating the adhesive fluorocarbon resin sheet 5 on the glass substrate 3, or by laminating the glass substrate 1 on the fluorocarbon resin body 27 so that one end of the flow path 7 is aligned with the through hole 9 and the other end of the flow path 7 is aligned with the through hole 11. The flow cell according to the third embodiment has a metal film, such as platinum, formed by, for example, sputtering on the glass substrate 1 or the glass substrate 3 to further improve adhesion between the glass substrate and the fluorocarbon resin sheet 5 or between the glass substrate and the fluorocarbon resin body 27. By providing such a metal film on the surface of the glass substrate to be bonded to the fluorocarbon resin sheet 5 or the fluorocarbon resin body 27, it is possible to improve adhesion between the glass substrate and the fluorocarbon resin sheet 5 or between the glass substrate and the fluorocarbon resin body 27, thereby more effectively preventing the formation of a gap between members constituting the flow cell and therefore preventing liquid leakage.
Further, such a metal film can be patterned as shown in
For example, the electrode pattern 30 shown in
The present invention is not limited by the heating temperature, pressure, or flow path width described with reference to the preferred embodiments, and includes all embodiments within the scope of the appended claims.
The present invention can be applied to a flow cell constituting a flowmeter, an electric conductivity meter, or the like for use in an analytical instrument.
Filing Document | Filing Date | Country | Kind | 371c Date |
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PCT/JP2005/019562 | 10/25/2005 | WO | 00 | 4/23/2008 |