KR101401342B1 - Method for manufacturing multi-layered gas chromatography chip assembly obtained by multiple etching - Google Patents

Abstract

Disclosed are a method for manufacturing a gas chromatography chip through multi-etching and a method for manufacturing a chip laminate. The manufacturing of the gas chromatography chip via the etching comprises the steps of: (A) preparing an upper substrate and a lower substrate stage; (B) forming a micro-channel pattern; (C) forming a micro-channel; (D) forming a gas feed connection; (E) forming a gas discharge connection; (F) applying a fixed bed; and (G) manufacturing the gas chromatography chip.

Description

METHOD FOR MANUFACTURING MULTI-LAYERED GAS CHROMATOGRAPHY CHIP ASSEMBLY OBTAINED BY MULTIPLE ETCHING BACKGROUND OF THE INVENTION 1. Field of the Invention [0001]

The present invention relates to a method for producing a gas chromatography chip through multiple etching and a method for producing the same, and more particularly, to a gas chromatography chip obtained through multiple etching and a gas chromatography chip And a method of manufacturing a gas chromatography chip laminate.

Chromatography relates to analytical techniques that precisely separate each component from a simple mixture to a very complex mixture, i. E., A multicomponent mixture.

Chromatography can be divided into several types depending on the stationary phase and, in particular, the type of mobile phase.

Chromatography can be classified into gas chromatography and liquid chromatography depending on the type of the mobile phase. In the present invention, a description of liquid chromatography will be omitted.

In the gas chromatography technique, when a moving phase, in which a mixture is dispersed, is moved through a stationary phase, a moving phase Using features that leave traces.

That is, in the gas chromatography technique, the mixture to be separated is contained in the mobile phase.

The mixture component moves in a stationary phase, wherein each component of the mixture is separated while moving in the stationary phase.

At this time, gas chromatography is characterized in that it has a high resolution especially for volatile substances which are simple, fast, sensitive, and thermally stable.

Using chromatographic techniques, any mixture can be separated precisely for each component.

At this time, in the case of a gas chromatography chip in which a very complicated mixture is analyzed, there arises a difference in resolution depending on the total length of the microchannel, that is, the fixed phase and the polarity formed on the microchannel (stationary phase).

On the other hand, a conventional gas chromatography chip uses a dry reactive ion etching (DRIE) technique.

Here, a method of engraving a desired pattern on a substrate (wafer) will be briefly described.

In order to engrave a desired pattern on a substrate, (1) a substrate suitable for engraving a pattern is prepared, a thin film is formed on the substrate with a material suitable for etching, (2) a pattern Next, (3) an unnecessary portion of the thin film formed on the substrate can be removed by using an etching (etching) apparatus, so that a desired pattern can be formed in accordance with the pattern drawn in the design drawing.

This pattern engraving can be largely divided into a dry etching method and a wet etching method.

In the DRIE technique, an etching (etching) gas to be reacted with a wafer is made into a plasma state, and the etching gas of the plasma state is made to collide with the substrate to form a physical shock And a chemical reaction are bonded to each other, thereby etching a part of the substrate.

This dry etching technique has a problem in that it is difficult to implement due to the complexity of the apparatus and an excessive cost.

On the other hand, the wet etching technique is a technique for eliminating unnecessary portions of a thin film formed on a substrate surface by flowing a liquid chemical agent or a chemical substance on the surface of the substrate, and the implementation can be relatively simple and inexpensive as compared with the dry etching technique There are advantages.

A prior art related to the present invention is Korean Registered Patent No. 10-0243995 (issued Feb. 2, 2000).

Accordingly, it is an object of the present invention to provide a method for producing a gas chromatography chip using a transparent substrate and an inexpensive wet etching method.

At this time, since the microchannel of the desired depth can not be obtained through the single etching by the gas chromatography chip of the present invention using the transparent substrate, it is preferable to perform the multiple etching.

It is also an object of the present invention to provide a method for effectively sealing a substrate by bonding the substrate by a simple method.

The present invention also aims to control the polarity of the stationary phase formed on the microchannel on the substrate.

It is another object of the present invention to provide a gas chromatography chip laminate obtained by laminating multiple gas chromatography chips obtained through multiple etching as well as a single gas chromatography chip obtained by multiple etching.

The problems to be solved by the present invention are not limited to the above-mentioned problem (s), and another problem (s) not mentioned can be understood by those skilled in the art from the following description.

According to an aspect of the present invention, there is provided a method of manufacturing a gas chromatography chip by multi-etching comprising: (A) preparing an upper substrate and a lower substrate; (B) forming a microchannel pattern portion on one surface or both surfaces of the upper substrate or the lower substrate facing each other; (C) etching the microchannel pattern portions three or more times to form microchannels; (D) forming a gas supply connection portion on a surface opposite to the surface of the substrate on which the microchannel pattern portion is formed; (E) forming a gas discharge connection on a surface opposite to the substrate surface on which the microchannel pattern portion is formed, or on an opposite surface of the counterchief substrate on which the microchannel pattern portion is not formed; (F) applying a stationary phase on the inner surface of the substrate on which the microchannel pattern is formed by spin coating; And (G) preparing a gas chromatography chip by joining opposing surfaces of a substrate on which the stationary phase is applied and a substrate on which the stationary phase is not coated, the microchannel pattern portion having a circular cross section And a microchannel extending continuously from the gas supply connection to the gas discharge connection; Wherein the gas supply connection portion is formed in a tapered shape in which the width of the gas supply connection portion is narrow as the gas supply port side is advanced to the microchannel; One or more alignment markers are formed on opposing inner surfaces of the upper substrate or the lower substrate; And a temperature control unit and a temperature control unit for controlling the temperature of the substrate; Wherein the gas supply connection part and the gas discharge connection part are formed by an EDM method or a sandblast method; The temperature control device performs temperature control of the substrate and simultaneously applies a thermal pressure to the substrate to prevent gas loss in the microchannel formed in the substrate.

Here, it is preferable that the material of the substrate is one selected from a glass wafer, a quartz wafer, a polydimethylsiloxane wafer, a silicon wafer, a silicate wafer, a borosilicate wafer, and a fused silica wafer.

In addition, in the step (F), the fixed phase may be PDMS, and further, one selected from silica gel, alumina, char, molecular sieve, and porous polymer may be further coated to control the polarity of the microchannel Do.

The step (F) may further include sealing the bonding surface of the substrate when the upper substrate and the lower substrate are bonded to each other.

According to the present invention, a gas chromatography chip obtained by a method of manufacturing a gas chromatography chip by multiple etching is used for forming a gas discharge connection portion of a preceding gas chromatography chip and a gas supply connection portion of a following gas chromatography chip to each other And a length of the microchannel is extended by connecting the microchannel to the microchannel.

Here, the stationary phase further coated on the stationary phase of the gas chromatography chip may be different for each layer of the gas chromatography chip laminate.

The details of other embodiments are included in the detailed description and the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS The advantages and / or features of the present invention and the manner of achieving them will be apparent from and elucidated with reference to the embodiments described hereinafter in conjunction with the accompanying drawings.

It should be understood, however, that the invention is not limited to the disclosed embodiments, but may be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. The present invention is not intended to be exhaustive or to limit the invention to the precise form disclosed, and it is to be understood that the invention is limited only by the terms of the appended claims.

It is to be understood that the same reference numerals refer to the same components throughout the specification and that the size, position, coupling relationship, etc. of each component constituting the invention may be exaggerated for clarity of description.

As described above, according to the method for producing a gas chromatography chip by multi-etching according to the present invention and the method for producing the above-mentioned chip-stacked body, it is economically advantageous to manufacture a gas chromatography chip by a wet etching method.

Further, according to the present invention, the gas chromatography chips obtained by the present invention are bonded and sealed in a simple and efficient manner when bonding the substrates.

Further, according to the present invention, the gas chromatography chip obtained by the present invention can control the polarity of the stationary phase coated on the microchannel.

Further, according to the present invention, it is possible to provide a gas chromatography chip laminate obtained by laminating a plurality of gas chromatography chips obtained by the present invention.

1 is a flowchart schematically showing a method of manufacturing a gas chromatography chip by multiple etching according to a preferred embodiment of the present invention.
Figure 2 is a schematic top view of a gas chromatography chip obtained through multiple etching, in accordance with a preferred embodiment of the present invention.
FIG. 3 is a table showing the depth of etching of a substrate during multiple etching, according to a preferred embodiment of the present invention.
4 (a) is a view showing the same shape of a flow path of a gas inflow path of a gas supply connection portion of a gas chromatography chip according to a preferred embodiment of the present invention, and Fig. 4 (b) Sectional view of a gas supply connection portion of a gas chromatography chip obtained through multiple etching according to a preferred embodiment of the present invention, in which the channel width of the gas inlet connection portion is tapered.
FIG. 5 is a partially enlarged view showing the configuration of a gas supply connection portion of the gas chromatography chip, together with a schematic plan view of a gas chromatography chip obtained through multiple etching according to a preferred embodiment of the present invention.
Figure 6 is a photograph of a gas supply connection, a microchannel, and a gas discharge connection of a gas chromatography chip obtained through multiple etching, according to a preferred embodiment of the present invention, Fig. 3 is a view showing a state of a gas supply / discharge connector; Fig.
FIG. 7 is a graph showing the results of actual gas analysis of a gas chromatography chip obtained through multiple etching according to a preferred embodiment of the present invention. In the figure, ECD detection results of chloroform and 4-bromofluorobenzene are shown.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

It should be noted that the terms 'coating' and 'coating', 'wafer' and 'substrate', and 'etching' and 'etching', respectively, are used in the present invention in substantially the same sense.

Hereinafter, a method of manufacturing a gas chromatography chip by multiple etching according to a preferred embodiment of the present invention will be described with reference to FIG.

1 is a flowchart schematically showing a method of manufacturing a gas chromatography chip by multiple etching according to a preferred embodiment of the present invention.

1, a method of manufacturing a gas chromatography chip by multiple etching according to a preferred embodiment of the present invention includes a substrate preparation step S100, a pattern formation step S110, an etching step S120, , A fixed-phase coating step (S130), and a substrate bonding step (S140).

Substrate preparation

The substrate preparation step (S100) is a step of preparing a substrate to be used in a method of manufacturing a gas chromatography chip by multiple etching according to a preferred embodiment of the present invention.

The substrate is preferably one selected from the group consisting of a glass wafer, a quartz wafer, a polydimethylsiloxane wafer, a silicon wafer, a silicate wafer, a borosilicate wafer, and a fused silica wafer, desirable.

Further, the substrate is preferably a standard 4 inch size, but the size of the substrate may be different if necessary.

Here, the substrate is preferably divided into an upper substrate and a lower substrate.

Naturally, the thickness of the substrate is not limited.

In addition, it is preferable to form an Au / Cr deposited film in advance on the substrate to be used in the method for manufacturing a gas chromatography chip by multiple etching according to a preferred embodiment of the present invention.

As the substrate on which a vapor deposition film is to be formed, the upper substrate and the lower substrate are not specified.

Since this vapor-deposited film can withstand hydrofluoric acid, it can contribute to effective etching in a wet etching described later.

As the deposition equipment used for forming the deposition film, an E-Beam Evaporator (Model: ei-5, manufacturer: ULVAC) was used. The thickness of the Cr film deposited first was about 200 to 300 Å, It is preferable that the thickness of the Au film deposited thereon is about 2000 angstroms.

Pattern formation

The pattern formation step (S110) is a step of forming a pattern to be formed on the prepared substrate.

The pattern referred to in this step S110 indicates a pattern similar to that shown in Fig. 2. It is preferable that a pattern is formed in advance by using a pattern forming program.

As a specific example of pattern formation, a pattern similar to that shown in Fig. 2 is formed in advance by using a pattern forming program, and this pattern is printed on a blank master (model name: Photo Plotter Mask, manufactured by Barco) , And a method of forming the blank master by etching (etching) the substrate 10 using the blank master as a photomask used for patterning the substrate 10 (FIG. 2) of the present invention.

A person skilled in the art can form a desired pattern on the substrate 10 using a photomask and a photoresist applied on the substrate 10, .

SU-850 (manufactured by Microchem, USA) can be used as the photoresist.

The SU-850 is a photoresist for negative etching, and the thickness of the coating may be adjusted to 40 to 100 m.

In addition, it is preferable that alignment markers for the purpose of facilitating alignment at the time of etching the substrate are also formed at the same time.

A more detailed pattern formation method will be described later.

etching

The etching step (S120) is a step of etching the substrate in a predetermined pattern shape.

In the etching step (S120), it is preferable to etch only the pattern formed on the substrate.

At this time, etching can be performed by applying the photoresist PR and the wet etching method using the photomask having the desired pattern formed therein.

In this etching step (S120), it is preferable that the wet etching is repeated at least three times or more until a desired etching depth, that is, about 50 탆 is obtained. This will be described later with reference to FIG.

Fixed application

The step of applying a fixed phase (S130) is a step of applying a fixed phase, preferably PDMS (Polydimethylsiloxane), to the surface of the etched substrate in the etching step (S120).

The PDMS was optically transparent, non-polar, non-flammable and was applied by spin coating using a spin coater. The specific spin coating method will be described in more detail in the following paragraphs of the embodiments.

For reference, it should be noted that the substrate used in the present invention is also optically transparent.

In the present stationary phase application step (S130), in addition to the above-described PDMS, a stationary phase having a different polarity may be further applied to the coating layer of the substrate, if necessary.

Examples of stationary phases having different polarities include silica gel, alumina, charcoal, molecular sieve, and porous polymer, and when they are applied in a stationary phase, the polarity of the microchannel can be easily controlled.

Substrate junction

The substrate bonding step (S140) is a step of bonding the substrate on which the application of the fixed phase has been completed.

At this time, it should be noted that the PDMS coated on one surface of the upper substrate or the lower substrate constituting the substrate not only functions as a fixed phase but also acts to bond the substrate of the present invention.

Thus, the PDMS can contribute to the role of the stationary phase in the microchannel, and the sealing between the upper substrate and the lower substrate at the same time.

Alternatively, the PDMS may be coated on both surfaces of the upper substrate and the lower substrate.

Here, the PDMS does not use a method of coating the wall surface of the microchannel by pressurizing and injecting into one of the openings of the microchannel after joining the upper substrate and the lower substrate, but using a spin coating method using a spin coater It should be noted that it can be applied very simply by a coating method.

Next, Fig. 2 is a schematic plan view of a gas chromatography chip obtained through multiple etching, according to a preferred embodiment of the present invention.

Here, the gas chromatography chip includes a substrate 10 formed in a circular shape, alignment markers 20 and 30 formed on one surface of the substrate 10, a gas supply device for supplying gas to the gas chromatography chip A microchannel 60 and a microchannel 60 to cover most of the plane of the substrate 10 starting from one side of the substrate 10, And a microchannel pattern portion 70 in which a channel 60 is extended.

The substrate 10 may be divided into an upper substrate and a lower substrate as described above and the gas supply connection portion 40, the gas discharge connection portion 50, the microchannel 60, (70) may be formed on either one of the upper substrate and the lower substrate, respectively.

Alternatively, only a part of these components may be formed on either side of the upper substrate and the lower substrate of the substrate 10, and the remaining part may be formed on the opposite surface of the substrate 10 opposite the upper substrate and the lower substrate It is possible.

The material of the substrate 10 is preferably one selected from the group consisting of a glass wafer, a quartz wafer, a polydimethylsiloxane wafer, a silicon wafer, a silicate wafer, a borosilicate wafer, and a fused silica wafer, Is most preferable.

Although the alignment markers 20 and 30 are shown on both sides of the substrate 10 facing the substrate 10 with the microchannel pattern portion 70 interposed therebetween , The positions of the alignment markers 20 and 30 are not limited thereto.

That is, the positions of the alignment markers 20 and 30 may be formed on one surface of the substrate 10 or on one surface and the other surface of the substrate 10, have.

Accordingly, an alignment marker may be formed adjacent to one side of the substrate 10, or alternatively, only one side of the substrate 10 may be formed on one side of the substrate 10, It is also possible to use this cut face as an auxiliary positioning marker after cutting.

In the drawing, the gas supply connection portion 40 is formed on one side of the upper end of the substrate 10, but the formation position may be any other position.

The gas supply connection portion 40 is a portion used for supplying the mixture gas as a mobile phase to the gas chromatography chip obtained according to the preferred embodiment of the present invention.

A gas supply side connector 80 and a gas supply column 100 (see FIG. 6) are connected to a gas supply side of the gas supply connection unit 40, Gas is supplied. At this time, a gas supply side connector 80 (see FIG. 6) is preferably provided between the substrate 10 and the gas supply column 100.

The gas supplied to the gas supply connection portion 40 flows into the microchannel 60 formed continuously.

The microchannel 60 is a microchannel constituting the microchannel pattern unit 70 and serves to continuously flow the gas of the mobile phase that has flowed from the gas supply connection unit 40.

The microchannel pattern portion 70 preferably has a pattern formed in advance by using a pattern forming program. As described above, the pattern is printed on a blank master, and the blank master is transferred to the substrate 10 And the substrate 10 is etched by using the photomask as a photomask.

The microchannel pattern portion 70 formed in accordance with the preferred embodiment of the present invention has a width of about 100 mu m.

Therefore, it is obvious that the width of the microchannel 60 formed on the substrate 10 is formed to have substantially the same width.

On the other hand, the length of the microchannel 60 formed on the substrate 10 can be increased or decreased according to the pattern shape of the microchannel pattern portion 70.

The gas discharge connection portion 50 is formed in a direction opposite to the extending direction of the gas supply connection portion 40 formed at one side of the upper end of the substrate 10, but the present invention is not limited thereto.

Although the gas supply connection portion 40 and the gas discharge connection portion 60 are shown in the shape of "┑" and "┎" respectively in the drawing, the gas supply connection portion 40 and the gas discharge connection portion 60 (50) may be formed so as to face each other like the shapes of "┎" and "┑".

The gas supply connection portion 40 and the gas discharge connection portion 50 may be formed collectively on one side surface of the substrate 10 but may be formed on the upper side and the lower side or the right side and the left side of the substrate 10, Or may be formed spaced apart.

Alternatively, the gas supply connection portion 40 and the gas discharge connection portion 50 may be formed on one surface of the substrate 10, and another one may be formed on the opposite surface of the substrate 10 .

The gas discharge connection portion 50 is a portion through which gas as a mobile phase supplied to the gas chromatography chip obtained according to the preferred embodiment of the present invention is discharged.

A gas discharge side connector 90 and a gas discharge column 110 (refer to FIG. 6) are connected to a gas discharge side of the gas discharge connection portion 50. The gas discharge side connector 90 and gas The mobile phase gas is discharged through the discharge column (110).

The gas discharged from the gas discharge connection part 50 may be discharged to the outside. Alternatively, when a gas chromatography chip stack is formed by stacking gas chromatography chips, (Not shown) of another gas chromatography chip adjacent or at a remote site.

That is, the gas discharged from the gas discharge side connector provided at the gas discharge connection portion of the preceding gas chromatography chip can be continuously supplied to the gas supply side connector provided at the gas supply connection portion of the following gas chromatography chip.

In the gas chromatography technique, temperature control of the entire apparatus is very important. In particular, in order to analyze the mixture with high resolution, it is necessary to precisely control the temperature of the microchannel 60 formed in the substrate 10 and the substrate 10 have.

Although not shown in the drawings, the positioning markers 20 and 30, the gas supply connection portion 40, the gas discharge connection portion 50, and the microchannel 60, which are formed on the substrate 10, A heat transfer portion may be formed at a portion except for the portion 70. [

Alternatively, the heat transfer part (not shown) may heat the entirety of the gas supply connection part 40, the gas discharge connection part 50, and the microchannel 60 and the microchannel pattern part 70 formed on the substrate 10 As shown in FIG.

Further, in this case, it is more preferable that a temperature control device (not shown) is additionally provided in the heat transfer portion.

In the case of the gas chromatography chip according to the present invention, the temperature of the gas chromatography chip can be controlled at high speed and precisely by the temperature control device.

At this time, a peltier element may be used in consideration of the small size of the substrate 10 in the heat transfer part.

FIG. 3 is a table showing the depth of etching of a substrate during multiple etching, according to a preferred embodiment of the present invention.

3, when the etching was performed once, the depth of the microchannel 60 was about 17 탆 to 20 탆 (average depth: 18 탆), but when the etching was performed three times, And the depth of the surface 60 is deepened to about 42 탆 to about 57 탆 (average depth: 50 탆).

In the preferred embodiment of the present invention, the depth of the microchannel 50 formed was 50 탆.

4 (a) is a view showing the same shape of a flow path of a gas inflow path of a gas supply connection portion of a gas chromatography chip according to a preferred embodiment of the present invention, and Fig. 4 (b) Sectional view of a gas supply connection portion of a gas chromatography chip obtained through multiple etching according to a preferred embodiment of the present invention, in which the channel width of the gas inlet connection portion is tapered.

The gas supply channel shown in FIG. 4A is formed in parallel with the channel itself. In the gas supply channel shown in FIG. 4B, the channel itself has a width of a portion of the gas supply port It can be seen that a flow path is formed in which the width is widest and the width becomes narrower toward the right side.

In the present invention, the shape of the gas inflow path of the gas supply connection portion is formed in a tapered shape when the parallel flow path is formed as shown in FIG. 4 (a) And the amount of gas discharged to the gas discharge connection portion 50 of the substrate 10 is too small.

4B, the gas supply port side is formed to have a width of about 500 mu m and the width of the microchannel pattern portion 70 is reduced to about 100 mu m to the start point of the microchannel 60, Tapered shape.

The specific shape thereof will be described with reference to Fig.

FIG. 5 is a partially enlarged view showing a configuration of a gas supply connection portion of the gas chromatography chip, together with a schematic plan view of a gas chromatography chip obtained through multiple etching according to a preferred embodiment of the present invention. FIG.

5, the width of the flow passage near the gas supply port 42 formed in the gas supply connection portion 40 of the gas chromatography chip according to the preferred embodiment of the present invention is about 500 μm, Since the width of the flow path far from the gas supply port 42 is about 100 탆, they form the tapered channel portion 44.

Figure 6 is a photograph of a gas supply connection, a microchannel, and a gas discharge connection of a gas chromatography chip obtained through multiple etching, according to a preferred embodiment of the present invention, Fig. 3 is a view showing a state of a gas supply / discharge connector; Fig.

6, in the gas chromatography chip according to the preferred embodiment of the present invention, the gas supply side connector 80 is provided in the gas supply port 42 of the gas supply connection portion 40 formed on one side of the substrate 10 And the gas discharge side connector 90 is provided in the gas discharge port (not shown) of the gas discharge connection part 50 formed on the other side of the substrate 10. [

In the preferred embodiment of the present invention, the Nanoport Assembly (R) (Upchurch Scientific (USA)) is used as the gas supply side connector 80 and the gas discharge side connector 90, ether ketone), it satisfies the desired heat-resistant condition (mp = 340 ° C), and even when high pressure is applied to the gas chromatography chip, gas outflow from the inside of the substrate 10 does not occur.

7 is a graph showing the results of actual gas analysis of a gas chromatography chip obtained through multiple etching according to a preferred embodiment of the present invention. In the figure, ECD detection results of chloroform and 4-bromofluorobenzene are shown Respectively.

In order to obtain the graph of FIG. 7, 9 μl of chloroform and 1 μl of 4-bromofluorobenzene were mixed as an analytical sample, and then hexane (Hexane) .

As the analysis equipment, a μECD detector (model: HP 6890, manufacturer: Agilent, USA) was used.

Other conditions for analysis are as follows.

Gas supply temperature: 300 ° C

Carrier gas: He

Pressure: 1.30 MPa

Split ratio: 50: 1

Feed amount: 1 μl

Column used: Micro fab column (2 m x 0.10 mm ID x 0.1 mu m)

Temperature ramp: 40 ° C (2 min) → 10 ° C / min → 120 ° C (10 min)

Detector temperature: 300 ° C

As can be seen in FIG. 7, the first peak in the graph clearly indicates chloroform, and the second peak in the graph clearly indicates 4-bromofluorobenzene.

Next, a method of manufacturing a gas chromatography chip according to a preferred embodiment of the present invention and a method of implementing the laminated body will be described.

In this regard, it should be understood that the description has been described with reference to FIG. 1, and the description may be omitted or the description may be omitted for the parts already described.

First, a substrate made of an upper substrate and a lower substrate is prepared.

At this time, the material of the substrate is preferably one selected from a glass wafer, a quartz wafer, a polydimethylsiloxane wafer, a silicon wafer, a silicate wafer, a borosilicate wafer and a fused silica wafer, and most preferably a borosilicate wafer.

As described above, a photoresist (PR) and a wet etching method are applied to the borosilicate wafer using a mask having a desired pattern to form a microchannel pattern portion having a width of about 100 mu m.

The width of the microchannel in the mask was 0.1 mm, the diameter of the gas supply connection and the gas discharge connection was 0.5 mm, and the length of the entire microchannel was 6054 mm.

As described above, the wet etching at this time is preferably repeated at least three times or more until a desired etching depth, that is, about 50 탆 is obtained.

The microchannel 60 or the microchannel pattern unit 70 may be formed on one side of one of the upper and lower substrates constituting the substrate 10 or on both sides of the other substrate Lt; / RTI >

Since the etching is repeated with reference to the positioning markers 20 and 30 formed on the substrate 10 as described above, the microchannel 60 and the microchannel pattern portion 70 of a desired pattern can be formed with a predetermined depth and width And also can be etched to interlock with each other.

As a result, the cross section of the microchannel 60 to be obtained can be a circular shape.

As described above, since the masking layer and other special equipment, which were necessary in the conventional DRIE technique, are not required, the microchannel pattern portion 70 is formed on the substrate 10 in a simple manner at a low cost by using the above- can do.

Next, PDMS (Polydimethylsiloxane) is applied as a fixed phase and for bonding / sealing the upper substrate and the lower substrate.

At this time, PDMS was optically transparent, non-polar and non-flammable, and was applied by spin coating using a spin coater.

The rotation speed of the spin coater during spin coating was about 4000 to 8000 RPM and the rotation duration was about 1 second.

Also, in order to lower the viscosity of PDMS, it was diluted with toluene at a ratio of 1: 1 or 1: 2 (v / v), so that the coating height of PDMS was also suppressed to the maximum level.

According to an embodiment of the present invention, spin coating is applied to only one surface of the upper substrate or the lower substrate constituting the substrate 10, and both substrates of the upper substrate and the lower substrate are bonded to each other without application to the other surface. , And heated in an oven at a temperature of 70 DEG C for about 1 hour to complete the bonding.

At this time, it is preferable that the PDMS is coated on either one side of the upper substrate or the lower substrate which forms the substrate, or alternatively, it may be coated on both sides.

This coated PDMS can contribute to the sealing between the substrate 10 and the flow of gas in the microchannel 60 because it can be used directly for the bonding of the silicate wafer as well as for the function of the stationary phase.

That is, the PDMS is a technically difficult method for coating the wall surface of the microchannel 60 by pressurizing and injecting gas into either the gas supply connection part 40 or the gas discharge connection part 50 after forming the gas chromatography chip However, it can be fabricated by a simple coating method using a spin coater, which is very economical.

Here, as described above, if necessary, a fixed phase having a different polarity may be further applied to the coating layer of the substrate 10. [

Examples of stationary phases having different polarities include silica gel, alumina, charcoal, molecular sieve, and porous polymer. When they are applied in a fixed phase, the polarity of the microchannel 60 can be easily controlled.

In addition, the fixed phase having different polarities may be applied to either the upper substrate or the lower substrate of the substrate 10, or may be applied to the entire microchannel 60.

Furthermore, in the case of forming a gas chromatography chip laminate, the same stationary phase may be applied to each gas chromatography chip, or a different stationary phase may be applied to each gas chromatography chip.

As described above, since the chip fabrication in the preferred embodiment of the present invention uses a wet etching technique unlike the conventional dry etching technique (DRIE), it is possible to use an inexpensive and simple structure spin coater, But it is economically effective.

According to a preferred embodiment of the present invention, the specifications of the substrate 10 used in the gas chromatography chip are as follows.

Size of substrate: 4 inches

Size of gas inlet: 500 ㎛

Size of gas outlet: 500 ㎛

Width of microchannel: 100 탆

Substrate material: Borosilicate wafer

It should be noted that the size of the gas supply port is 500 mu m and the width of the microchannel is 100 mu m so that the flow path from the gas supply port to the microchannel is tapered.

Next, a method of forming a gas outlet (not shown) formed in the gas supply port 42 and the gas discharge connection portion 50 formed in the gas supply connection portion 40 of the gas chromatography chip according to a preferred embodiment of the present invention .

First, the gas supply port and the gas discharge port can be precisely realized by sandblasting, but the sandblasting method is very inefficient in order to produce a small amount of gas. Therefore, according to a preferred embodiment of the present invention, The gas outlet was fabricated using an electrical discharge machining (EDM) technique.

At this time, a 5 M KOH solution was prepared. Then, the gas chromatography chip of the present invention was thoroughly immersed in the KOH solution (immersed for 8 mm or more), and a current of 40 V / 3 A was flowed.

The electrodes and the solution for electric discharge machining were appropriately exchanged as necessary.

The gas supply port and the gas discharge port may be formed simultaneously on one side of the gas chromatography chip, one of them may be formed on one side, and the other may be formed on the other side.

In the case of the former, there is an advantage that the operation is convenient. In the latter case, it can be very advantageous when forming the gas chromatography chip laminate.

 Next, a column for supplying the gas mixture to be analyzed is connected to the gas chromatography chip obtained according to the preferred embodiment of the present invention.

6, the gas supply side connector 80 is installed in the gas supply port 42 of the gas supply connection portion 40 formed on one side of the gas chromatography chip according to the preferred embodiment of the present invention , And a gas discharge side connector (90) is provided in a gas discharge port (not shown) of the gas discharge connection part (50) formed on the other side of the chip.

The gas supply side connector 80 and the gas discharge side connector 90 may be connected to a gas supply column 100 and a gas discharge column 110 respectively for supplying gas from the outside.

The gas supply column 100 is a column for supplying a mobile phase gas and a gas containing a mixture to be analyzed, and the gas discharge column 110 discharges the gas to the outside, Is connected to the gas supply connection of the other gas chromatography chip.

In addition, the application of PDMS, the bonding of the substrate, the deposition of Au / Cr, and the like have been described above, and therefore, the description thereof is omitted.

The analysis performance of the gas chromatography chip according to the preferred embodiment of the present invention, which has been produced as described above, has also been described with reference to FIG.

Here, in order to measure the analytical performance of the gas chromatography chip obtained according to the method for producing the gas chromatography chip through the multiple etching of the present invention and the method for producing the chip laminate, the detection connected to the gas chromatography chip Apparatus, for example, a flame ionization detector (FID), an electron capture detector (ECD), and a mass spectrometer.

ECD is mainly useful for the detection of compounds containing halogen elements (eg F, Cl, Br, I) and is mainly used for the detection of pesticides, PCB, N ₂ O gas and the like. FID is mainly used for the analysis of organic compounds such as HC, TCE and PCE.

In addition, the gas chromatography chip obtained according to the preferred embodiment of the present invention may further include a heat transfer portion for temperature control as described above.

The heat transfer part may be formed in an area where the accessory of the gas chromatography chip is not formed, or may be formed so as to heat the entire gas chromatography chip.

In addition, as described above, it is preferable that a temperature control device is further provided in the heat transfer portion.

Therefore, in the case of the gas chromatography chip according to the present invention, since the temperature of the gas chromatography chip can be controlled at high speed and precisely by the temperature control device, the temperature can be controlled instantaneously compared with the conventional gas chromatography technique So that a very sharp peak can be obtained in the analysis of the gas mixture.

At this time, the heat transfer part may use a peltier element in consideration of the small size of the gas chromatography chip.

The heat transfer part controls the temperature of the gas chromatography chip, and at the same time, acts to prevent gas loss in the microchannel by applying thermal pressure to the junction between the upper substrate and the lower substrate constituting the gas chromatography chip.

This is because the heat applied to the gas chromatography chip enhances the adhesion of the PDMS applied between the upper substrate and the lower substrate.

While the present invention has been described in connection with what is presently considered to be practical exemplary embodiments, it is to be understood that the invention is not limited to the disclosed embodiments.

Therefore, the scope of the present invention should not be limited to the described embodiments, but should be determined by the scope of the appended claims and equivalents thereof.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, Modification is possible.

Accordingly, the spirit of the present invention should be understood only in accordance with the following claims, and all equivalents or equivalent variations thereof are included in the scope of the present invention.

S100: Substrate preparation step
S110: pattern formation step
S120: etching step
S130: Fixed phase application step
S140: Substrate bonding step
10: substrate
20, 30: Position alignment marker
40: gas supply connection
42: gas supply port
44: tapered channel part
50: gas discharge connection
60: Microchannel
70: Microchannel pattern portion
80: gas supply side connector
90: Gas discharge side connector
100: gas supply column
110: gas discharge column

Claims (6)

(A) preparing an upper substrate and a lower substrate;
(B) forming a microchannel pattern portion on one surface or both surfaces of the upper substrate or the lower substrate facing each other;
(C) etching the microchannel pattern portions three or more times to form microchannels;
(D) forming a gas supply connection portion on a surface opposite to the surface of the substrate on which the microchannel pattern portion is formed;
(E) forming a gas discharge connection on a surface opposite to the substrate surface on which the microchannel pattern portion is formed, or on an opposite surface of the counterchief substrate on which the microchannel pattern portion is not formed;
(F) applying a stationary phase on the inner surface of the substrate on which the microchannel pattern is formed by spin coating; And
(G) preparing a gas chromatography chip through multiple etching by joining the opposite side of the substrate on which the stationary phase is not applied and the side of the substrate on which the stationary phase has been applied,
Wherein the microchannel pattern portion has a circular cross section and is formed of a microchannel continuously extending from the gas supply connection portion to the gas discharge connection portion;
Wherein the gas supply connection portion is formed in a tapered shape in which the width of the gas supply connection portion is narrow as the gas supply port side is advanced to the microchannel;
One or more alignment markers are formed on opposing inner surfaces of the upper substrate or the lower substrate;
Wherein the gas supply connection part and the gas discharge connection part are formed by an EDM method or a sandblast method;
The gas chromatography chip through the multiple etching is connected to the gas discharge connection portion of the preceding gas chromatography chip and the gas supply connection portion of the following gas chromatography chip to form a gas chromatograph A method of manufacturing a laminated graphical chip,
Characterized in that the stationary phase further coated on the stationary phase may be different for each layer of the gas chromatographic chip laminate,
A method for producing a gas chromatographic chip laminate through multiple etching.
The method according to claim 1,
The material of the substrate is,
Wherein the substrate is one selected from the group consisting of glass wafers, quartz wafers, polydimethylsiloxane wafers, silicon wafers, silicate wafers, borosilicate wafers, and fused silica wafers.
A method for producing a gas chromatographic chip laminate through multiple etching.
3. The method of claim 2,
In the step (F), the stationary phase is PDMS,
Further comprising coating a selected one of silica gel, alumina, char, molecular sieve, and porous polymer as a stationary phase further coated on the stationary phase to control the polarity of the microchannel.
A method for producing a gas chromatographic chip laminate through multiple etching.
The method of claim 3,
Wherein the step (F) further comprises the step of sealing the joint surface of the substrate when the upper substrate and the lower substrate are bonded to each other.
A method for producing a gas chromatographic chip laminate through multiple etching.
The method according to claim 1,
Further comprising: a heat transfer unit and a temperature control device for controlling the temperature of the substrate;
Wherein the temperature control device performs temperature control of the substrate and simultaneously applies thermal pressure to the substrate to prevent gas loss in the microchannel formed in the substrate.
A method for producing a gas chromatographic chip laminate through multiple etching. delete

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