KR20240034360A - Column For Gas Chromatography And Method For Manufacturing Thereof - Google Patents

Abstract

The present invention relates to a column for gas chromatography and a method of manufacturing the same. More specifically, the column itself is made of a stationary phase material, so there is no need for a process to form a stationary phase material, and the column is manufactured by using a mold when manufacturing the column. It relates to a column for gas chromatography that can be more easily mass-produced and a method of manufacturing the same.

Description

Column for gas chromatography and method for manufacturing the same {Column For Gas Chromatography And Method For Manufacturing Thereof}

The present invention relates to a column for gas chromatography and a method of manufacturing the same. More specifically, the column itself is made of a stationary phase material, so there is no need for a process to form a stationary phase material, and the column is manufactured by using a mold when manufacturing the column. It relates to a column for gas chromatography that can be more easily mass-produced and a method of manufacturing the same.

Gas chromatography systems including samplers, pre-concentrators, columns, and detectors are being miniaturized according to user needs. The gas chromatography system separates each of the plurality of analytes from the sample by injecting the sample into a column whose inner wall is coated with a stationary phase material, thereby providing information on the components and concentrations of each of the plurality of analytes constituting the sample. Due to its unique characteristics, research on miniaturized columns with micro size is actively underway.

Patent Documents 1 to 4 disclose a gas chromatography system including a micro-sized column. Conventionally, in order to miniaturize the column, the column is manufactured by directly etching a substrate such as a wafer to form a channel and then closing the cover. However, this conventional method has a problem in that it requires very detailed work, like a semiconductor manufacturing process, and the workability is very poor, resulting in a very high production cost. In addition, the process of coating the stationary phase material on the inner wall of the column is very difficult, and many pores are created on the surface of the coated stationary phase material, so some of the analyte separated from the sample enters the inside of the pores and is injected into the detector. As the amount decreases, it may have a negative effect on analysis performance.

Considering this, Patent Document 5 discloses a technology that can relatively lower the production cost by using a polymer substrate. Specifically, Patent Document 5 forms a column by coating a stationary phase material on a polymer substrate and then closing the cover. However, this method still forms the shape of the channel by directly etching the substrate, which has the problem of not improving workability and increasing the production cost of the gas chromatography system.

Meanwhile, the applications for gas chromatography systems are gradually expanding. Recently, it has also been used for monitoring semiconductor manufacturing processes, as shown in Patent Documents 6 and 7. However, if a gas chromatography system with a high production cost is applied as in the past, it may also affect the production cost of the semiconductor manufacturing process, ultimately resulting in consumers using the product having to pay expensive product prices.

In other words, there is an urgent need to develop technology for gas chromatography columns that can be manufactured more easily while maintaining existing separation performance.

US published patent US2020-0033305 (Gas chromatography column with polybutadiene coating) U.S. published patent US2021-0300622 (Gas analyte spectrum sharpening and separation with multi-dimensional micro-gc for gas chromatography analysis) US registered patent US10,151,732 (Sealed micro gas chromatography columns and methods thereof) US published patent US2021-0172913 (Micro gas chromatography system) US published patent US2015-0219605 (Method for producing a chromatography analysis column) Korean patent application KR10-2021-0147802 (Measurement system for process monitoring) Korean patent application KR10-2021-0192770 (Measurement system for gaseous substances using multiple valves)

The present invention relates to a column for gas chromatography and a process for manufacturing the same, in which the column itself is made of a stationary phase material, so the process of forming the stationary phase material is not required, and the column can be more easily mass-produced by using a mold when manufacturing the column. The purpose is to provide a method.

In order to solve the above problems, an embodiment of the present invention provides a method of manufacturing a column for gas chromatography, comprising: preparing a mold including a pattern; Injecting a curable polymer material into a mold containing the pattern and curing it; removing the cured curable polymer material from the mold to form a superstructure; and placing a first substrate on the lower surface of the upper structure, and forming the gas chromatography column by bonding the upper structure and the first substrate to each other, wherein the gas chromatography column is inside the gas chromatography column. A method of manufacturing a column for gas chromatography is provided, in which a micro-passage having a height of 300 micrometers or less is formed.

In some embodiments of the invention, the curable polymer material may include polydimethylsiloxane (PDMS).

In some embodiments of the present invention, preparing a mold including the pattern includes forming a PR layer by spin-coating a negative photoresist on a second substrate; disposing a mask including through holes corresponding to the shape of the pattern on the PR layer; curing a portion of the PR layer by irradiating ultraviolet rays toward the mask; and removing another part of the PR layer using a developer, wherein a part of the PR layer may correspond to the pattern.

In some embodiments of the present invention, preparing a mold including the pattern includes forming a third substrate by 3D printing; and forming the pattern by 3D printing on the third substrate.

In some embodiments of the present invention, the column for gas chromatography may have a micro-passage formed inside the inner surface of the upper structure and a portion of the upper surface of the first substrate, and the micro-channel may be formed on the inner surface. The stationary phase material may be coated.

In some embodiments of the present invention, the column for gas chromatography may have a micro-passage formed inside the inner surface of the upper structure and a portion of the upper surface of the first substrate, and the micro-channel may be formed on the inner surface. A buffer layer is formed, and the upper surface of the buffer layer may be coated with a stationary phase material.

In some embodiments of the present invention, the stationary phase material may include an ionic liquid.

In some embodiments of the present invention, the pattern may include one of a spiral type and a parallel stacked type.

In order to solve the above problems, one embodiment of the present invention is a column for gas chromatography, comprising the steps of preparing a mold including a pattern; Injecting a curable polymer material into a mold containing the pattern and curing it; removing the cured curable polymer material from the mold to form a superstructure; and placing a first substrate on the lower surface of the upper structure and bonding the upper structure and the first substrate to form the gas chromatography column, wherein the gas chromatography column has an internal Provided is a column for gas chromatography in which a micro-passage having a height of 300 micrometers or less is formed.

In some embodiments of the invention, the curable polymer material may include polydimethylsiloxane (PDMS).

In some embodiments of the present invention, the column for gas chromatography may have a micro-passage formed inside the inner surface of the upper structure and a portion of the upper surface of the first substrate, and the micro-channel may be formed on the inner surface. The stationary phase material may be coated.

In order to solve the above problems, an embodiment of the present invention is a gas chromatography system including a column for gas chromatography, wherein the column for gas chromatography includes the steps of: preparing a mold including a pattern; Injecting a curable polymer material into a mold containing the pattern and curing it; removing the cured curable polymer material from the mold to form a superstructure; and placing a first substrate on the lower surface of the upper structure and bonding the upper structure and the first substrate to form the column for gas chromatography. It is manufactured through a process, and has a height of 300 micrometers or less inside. Provided is a gas chromatography system including a column for gas chromatography in which a micro-passage having a is formed.

In some embodiments of the invention, the curable polymer material may include polydimethylsiloxane (PDMS).

In some embodiments of the present invention, the column for gas chromatography may have a micro-passage formed inside the inner surface of the upper structure and a portion of the upper surface of the first substrate, and the micro-channel may be formed on the inner surface. The stationary phase material may be coated.

In order to solve the above problems, an embodiment of the present invention provides a method of manufacturing a gas chromatography system including a column for gas chromatography, comprising the steps of preparing a mold including a pattern; Injecting a curable polymer material into a mold containing the pattern and curing it; removing the cured curable polymer material from the mold to form a superstructure; and placing a first substrate on the lower surface of the upper structure, and forming the gas chromatography column by bonding the upper structure and the first substrate to each other, wherein the gas chromatography column is inside the gas chromatography column. A method of manufacturing a gas chromatography system including a column for gas chromatography in which a micro-passage having a height of 300 micrometers or less is formed is provided.

In some embodiments of the invention, the curable polymer material may include polydimethylsiloxane (PDMS).

According to one embodiment of the present invention, since the superstructure is formed with a curable polymer material, which is a type of stationary phase material, a separate process for forming the stationary phase material on the inner surface of the micro-channel is not required, thereby improving manufacturability. It can be effective.

According to an embodiment of the present invention, a superstructure is formed using a mold containing a pattern and bonded to a substrate to form a column, thereby enabling the mass production of multiple columns more easily and increasing productivity. can be demonstrated.

According to one embodiment of the present invention, when a stationary phase material is additionally coated on the inner surface of the micro-passage formed in the superstructure, pores formed relatively deeply in the micro-passage can be blocked, thereby improving the separation performance of the gas chromatography column. It can be effective.

According to one embodiment of the present invention, the effect of improving the pore treatment effect by the stationary phase material can be achieved by coating the inner surface of the micro-channel with a buffer material before coating the stationary phase material.

According to one embodiment of the present invention, the sample separation capacity of the gas chromatography column can be increased by increasing the surface area of the inner surface of the superstructure using a mold including a pattern with an increased surface area by plasma etching. can be demonstrated.

Figure 1 schematically shows a method of manufacturing a column for gas chromatography according to an embodiment of the present invention.
Figure 2 schematically shows an example in which a column for gas chromatography is manufactured according to an embodiment of the present invention.
Figure 3 schematically shows a plan view taken along line A-A' in Figure 2;
Figure 4 schematically shows detailed steps of preparing a mold including a pattern according to an embodiment of the present invention.
Figure 5 schematically shows an example in which a mold including a pattern according to an embodiment of the present invention is prepared.
Figure 6 schematically shows detailed steps of preparing a mold including a pattern according to another embodiment of the present invention.
Figure 7 schematically shows an example in which a mold including a pattern according to another embodiment of the present invention is prepared.
Figure 8 schematically shows detailed steps of preparing a mold including a pattern according to another embodiment of the present invention.
Figure 9 schematically shows an example in which a mold including a pattern according to another embodiment of the present invention is prepared.
Figure 10 conceptually shows an example of coating a stationary phase material on the inner surface of a micro-channel according to an embodiment of the present invention.
Figure 11 schematically shows a cross section of a superstructure and pores formed in the superstructure according to an embodiment of the present invention.
Figure 12 schematically shows an example of a superstructure according to an embodiment of the present invention.
Figure 13 schematically shows an example of a superstructure according to an embodiment of the present invention.
Figure 14 schematically shows an example of a superstructure according to an embodiment of the present invention.

BRIEF DESCRIPTION OF THE DRAWINGS Various embodiments and/or aspects are now disclosed with reference to the drawings. In the following description, for purposes of explanation, numerous specific details are set forth to facilitate a general understanding of one or more aspects. However, it will also be appreciated by those skilled in the art that this aspect(s) may be practiced without these specific details. The following description and accompanying drawings set forth in detail certain example aspects of one or more aspects. However, these aspects are illustrative and some of the various methods in the principles of the various aspects may be utilized, and the written description is intended to encompass all such aspects and their equivalents.

Additionally, various aspects and features may be presented by a system that may include multiple devices, components and/or modules, etc. It is also understood that various systems may include additional devices, components and/or modules, etc. and/or may not include all of the devices, components, modules, etc. discussed in connection with the drawings. It must be understood and recognized.

As used herein, “embodiments,” “examples,” “aspects,” “examples,” etc. may not be construed to mean that any aspect or design described is better or advantageous over other aspects or designs. .

Additionally, the term “or” is intended to mean an inclusive “or” and not an exclusive “or.” That is, unless otherwise specified or clear from context, “X utilizes A or B” is intended to mean one of the natural implicit substitutions. That is, either X uses A; X uses B; Or, if X uses both A and B, “X uses A or B” can apply to either of these cases. Additionally, the term “and/or” as used herein should be understood to refer to and include all possible combinations of one or more of the related listed items.

Additionally, the terms "comprise" and/or "comprising" mean that the feature and/or element is present, but exclude the presence or addition of one or more other features, elements and/or groups thereof. It should be understood as not doing so.

Additionally, terms including ordinal numbers, such as first, second, etc., may be used to describe various components, but the components are not limited by the terms. The above terms are used only for the purpose of distinguishing one component from another. For example, a first component may be named a second component, and similarly, the second component may also be named a first component without departing from the scope of the present invention. The term and/or includes any of a plurality of related stated items or a combination of a plurality of related stated items.

Additionally, the terms used in this specification are only used to describe specific embodiments and are not intended to limit the present invention. Singular expressions include plural expressions unless the context clearly dictates otherwise. In this specification, terms such as “comprise” or “have” are intended to indicate the presence of features, numbers, steps, operations, components, parts, or combinations thereof described in the specification, but are not intended to indicate the presence of one or more other features. It should be understood that this does not exclude in advance the possibility of the existence or addition of elements, numbers, steps, operations, components, parts, or combinations thereof.

In addition, in the embodiments of the present invention, unless otherwise defined, all terms used herein, including technical or scientific terms, are generally understood by those skilled in the art to which the present invention pertains. It has the same meaning as Terms defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the related technology, and unless clearly defined in the embodiments of the present invention, have an ideal or excessively formal meaning. It is not interpreted as

The column 1 for gas chromatography generally has a tube shape, and the inner surface of the tube is coated with a stationary phase material for separating a plurality of analytes constituting the sample. Conventionally, the column 1 for gas chromatography was manufactured by etching the surface of a substrate such as a wafer or polymer to form a channel and then covering the substrate with a cover.

However, this method requires fine work like a semiconductor manufacturing process in the process of forming the channel, and after covering, a separate work is required to coat the inner wall of the channel with a stationary phase material for material separation, making workability very difficult. There was a problem with the bad and high production cost.

In order to solve this problem, in the present invention, the column itself was formed from a stationary phase material.

Specifically, the present invention relates to a column (1) for gas chromatography and a method of manufacturing the same. A curable polymer material (200), which is a type of stationary phase material, is injected into a mold (100) in which a pattern (121) is formed and then cured to form a column. The main feature is to form a column 1 for gas chromatography by manufacturing a superstructure 300 and bonding the superstructure 300 to a substrate. At this time, the gas chromatography column 1 may have a micro-passage 320 formed by the pattern 121, and when a sample is injected into the micro-passage 320, the upper structure 300 may be formed. A plurality of analytes can be separated from the sample by the curable polymer material 200 (a type of stationary phase material).

In other words, the present invention is a gas chromatography column ( 1) and a method for manufacturing it can be provided.

Hereinafter, a column for gas chromatography (1) and a method of manufacturing the same according to an embodiment of the present invention will be described in detail.

Figure 1 schematically shows a method of manufacturing a column 1 for gas chromatography according to an embodiment of the present invention.

A method of manufacturing a column 1 for gas chromatography according to an embodiment of the present invention, comprising: preparing a mold 100 including a pattern 121 (S100); Injecting and curing a curable polymer material 200 into the mold 100 including the pattern 121 (S200); forming a superstructure 300 by removing the cured curable polymer material 200 from the mold 100 (S300); And placing a first substrate 400 on the lower surface of the upper structure 300, and bonding the upper structure 300 and the first substrate 400 to each other to form the gas chromatography column 1. Step (S400); may be included.

Step S100 shown in FIG. 1 corresponds to preparing the mold 100 including the pattern 121. In step S100, a pattern 121 capable of forming a passage through which a sample passes inside the column 1 for gas chromatography is formed on a substrate to prepare a mold 100 including the pattern 121. .

The pattern 121 corresponds to a configuration that forms an empty space inside the upper structure 300 to form a micro-passage 320 in the column 1 for gas chromatography. The micro-passage 320 corresponds to the channel of the column 1 for gas chromatography.

The step of preparing the mold 100 including the pattern 121 will be described in more detail with reference to the drawings described later.

Step S200 shown in FIG. 1 corresponds to injecting and curing the curable polymer material 200 into the mold 100 including the pattern 121. In step S200, the curable polymer material 200 can be molded by injecting the curable polymer material 200 into the mold 100 including the pattern 121 using a casting or injection method and then curing the mold 100 including the pattern 121.

The curable polymer material 200 corresponds to a type of stationary phase material, and preferably the curable polymer material 200 includes polydimethylsiloxane (PDMS). Polydimethylsiloxane (PDMS) is an OV1 series material and is a material suitable for use as a stationary phase that allows the analyte to be separated from the sample while the sample passes through the inside of the column 1 for gas chromatography.

In one embodiment of the present invention, the curable polymer material 200 can be cured by heating at a temperature of 40 to 60 degrees for 3 to 5 hours.

Step S300 shown in FIG. 1 corresponds to forming the upper structure 300 by removing the cured polymer material 200 from the mold 100. In step S300, the curable polymer material 200 molded and cured in step S200 is removed from the mold 100 to form the upper structure 300.

The upper structure 300 has a micro-passage 320 formed by the mold 100 including the pattern 121, and the micro-passage 320 may have a preset height. Preferably, the micro-passage 320 may have a height of 300 micrometers or less.

Step S400 shown in FIG. 1 places the first substrate 400 on the lower surface of the upper structure 300, and bonds the upper structure 300 and the first substrate 400 to each other for the gas chromatography. This corresponds to the step of forming column (1). In step S400, the upper structure 300 formed in step S300 is placed on one side of the first substrate 400 and then bonded, thereby finally forming the column 1 for gas chromatography.

In one embodiment of the present invention, the first substrate 400 may include a silicon wafer substrate.

That is, the column 1 for gas chromatography includes the upper structure 300 and the first substrate 400 bonded to each other. At this time, the upper structure 300 is manufactured through the steps S200 and S300, and a micro passage 320 with a height of 300 micrometers or less is formed therein, and the upper structure 300 including the micro passage 320 ) is bonded to the first substrate 400, the gas chromatography column 1 may include the micro-passage 320. Preferably, the gas chromatography column 1 according to an embodiment of the present invention has a micro-passage 320 formed therein with a height of 300 micrometers or less.

In this way, the method of manufacturing the column 1 for gas chromatography according to an embodiment of the present invention is to form the superstructure 300 with a curable polymer material 200, which is a type of stationary phase material, thereby forming the microchannel 320. There is no need for a separate process to form a stationary phase material on the inner surface, which has the effect of improving manufacturability.

Figure 2 schematically shows an example in which a column 1 for gas chromatography is manufactured according to an embodiment of the present invention.

The column 1 for gas chromatography according to an embodiment of the present invention includes preparing a mold 100 including a pattern 121 (S100); Injecting and curing a curable polymer material 200 into the mold 100 including the pattern 121 (S200); forming a superstructure 300 by removing the cured curable polymer material 200 from the mold 100 (S300); And placing a first substrate 400 on the lower surface of the upper structure 300, and bonding the upper structure 300 and the first substrate 400 to each other to form the gas chromatography column 1. It is manufactured through step (S400), and a micro-passage 320 having a height of 300 micrometers or less is formed inside the column 1 for gas chromatography.

As shown in FIG. 2, the column 1 for gas chromatography can be manufactured through the method of manufacturing the column 1 for gas chromatography described above.

More specifically, preparing a mold 100 including the pattern 121 (S100) and injecting a curable polymer material 200 into the mold 100 including the pattern 121 and curing it. The curable polymer material 200 may be injected into the mold 100 including the pattern 121 through (S200). At this time, the above steps are preferably performed with the mold 100 including the pattern 121 placed inside the open chamber 2 as shown in FIG. 2. Thereafter, the upper structure 300 formed through the step (S300) of removing the cured curable polymer material 200 from the mold 100 to form the upper structure 300, the upper structure 300 Through the step (S400) of placing a first substrate 400 on the lower surface of the gas chromatography column 1 and bonding the upper structure 300 and the first substrate 400 to each other, forming the column 1 for gas chromatography. By bonding to the first substrate 400, the gas chromatography column 1 according to an embodiment of the present invention can be formed. At this time, the upper structure 300 may have a channel groove 310 formed at the bottom by the pattern 121, and when the upper structure 300 is bonded to the first substrate 400, the channel groove ( A micro passage 320 may be formed in the upper structure 300 by blocking the lower portion of the first substrate 400 (310) by a portion of the first substrate 400.

Figure 3 schematically shows a plan view taken along line A-A' in Figure 2;

As shown in FIG. 3, the column 1 for gas chromatography according to an embodiment of the present invention has an upper structure 300 with a micro passage 320 formed therein, and is attached to one side of the first substrate 400. It may be formed by bonding the upper structure 300 and the first substrate 400 to each other. When a sample is injected into the column 1 for gas chromatography, the sample passes through the micro-passage 320 and undergoes a physical or chemical reaction with the inner surface of the upper structure 300 to produce a plurality of analyte substances. can be separated into

Since the column 1 for gas chromatography forms the upper structure 300 using a mold 100 including a pattern 121, the mold 100 used when forming the upper structure 300 The shape of the micro-passage 320 may be determined depending on the shape of the pattern 121. In one embodiment of the present invention, the pattern 121 may include one of a spiral type and a parallel stacked type.

For example, when forming the upper structure 300 by injecting and molding the curable polymer material 200 into the mold 100 including the pattern 121 having a spiral shape, the upper structure 300 The column 1 for gas chromatography may have a micro-passage 320 as shown in FIG. 3(a). In this case, the sample injected into the gas chromatography column (1) through the lower inlet of the gas chromatography column (1) passes through the micro-passage (320) and forms the upper structure (300). It can be separated into a plurality of analytes by siloxane (PDMS), and the plurality of analytes can be discharged from the gas chromatography column 1 through the lower inlet.

In addition, when the upper structure 300 is formed by injecting and molding the curable polymer material 200 into the mold 100 including the pattern 121 having a parallel stacked shape, the upper structure 300 includes the upper structure 300. The column 1 for gas chromatography may have a micro-passage 320 as shown in FIG. 3(b). In this case, the sample injected into the gas chromatography column (1) through the lower inlet of the gas chromatography column (1) passes through the micro-passage (320) and forms the upper structure (300). It can be separated into a plurality of analytes by siloxane (PDMS), and the plurality of analytes are released from the gas chromatography column (1) through the upper inlet of the gas chromatography column (1). You can. The operation of removing the upper structure 300 from the mold 100 including the pattern 121 having the parallel stacked shape of FIG. 3(b) includes the pattern having the spiral shape of FIG. 3(a) ( It can be performed relatively easily compared to the task of removing the upper structure 300 from the mold 100 including 121). This is due to the difference in shape of the pattern 121.

2 and 3, the gas chromatography column 1 according to an embodiment of the present invention includes a superstructure 300 manufactured using a mold 100 including a pattern 121. The main characteristic is that

In this way, in one embodiment of the present invention, the upper structure 300 is formed using the mold 100 including the pattern 121, and the upper structure 300 is bonded to the substrate to form a column, thereby making it easier to mass-produce a plurality of columns. It can be produced and have the effect of increasing productivity.

Figure 4 schematically shows detailed steps of preparing a mold 100 including a pattern 121 according to an embodiment of the present invention.

The detailed steps of preparing the mold 100 including the pattern 121 shown in FIG. 4 correspond to the step (S110) of preparing the mold 100 using a negative photoresist.

In the step (S110) of preparing the mold 100 using the negative photoresist, the mold 100 including the pattern 121 can be prepared by forming the pattern 121 on the substrate using the negative photoresist. there is.

Preferably, the step (S100) of preparing the mold 100 including the pattern 121 according to an embodiment of the present invention involves spin-coating a negative photoresist liquid on the second substrate 110 to form a PR layer ( 120) forming step (S111); Placing a mask 130 including through holes 131 corresponding to the shape of the pattern on the PR layer 120 (S112); Curing a portion 121 of the PR layer by irradiating ultraviolet rays toward the mask 130 (S113); and removing another part 122 of the PR layer using a developer (S114).

Step S111 shown in FIG. 4 corresponds to forming the PR layer 120 by spin coating a negative photoresist on the second substrate 110. In step S111, a first pretreatment operation is performed to form a pattern 121 on the second substrate 110 by coating the PR layer 120 on the second substrate 110 corresponding to the base portion of the mold 100. can do.

In one embodiment of the present invention, the negative photoresist may include SU-8 photoresist.

Step S112 shown in FIG. 4 corresponds to disposing a mask 130 including a through hole 131 corresponding to the shape of the pattern on the PR layer 120. In step S112, a secondary pretreatment operation to form the pattern 121 on the second substrate 110 can be performed by placing a mask 130 to cure a portion of the negative photoresist.

The mask 130 preferably includes through holes 131 corresponding to the shape of a pattern including one of a spiral type and a parallel stacked type.

Step S113 shown in FIG. 4 corresponds to curing a portion 121 of the PR layer by irradiating ultraviolet rays toward the mask 130. In step S113, the PR layer 120 formed on the second substrate 110 can be patterned using ultraviolet rays.

While part 121 of the PR layer may be hardened by the mask 130, the other part 122 of the PR layer may not be hardened.

Step S114 shown in FIG. 4 corresponds to removing another part 122 of the PR layer using a developer. In step S114, the photo process can be completed by removing the other part 122 of the PR layer that was not cured in step S113.

After step S114 is completed, the mold 100 in which a portion 121 of the PR layer is formed on the second substrate 110 can be prepared. At this time, part 121 of the PR layer corresponds to the pattern 121.

Figure 5 schematically shows an example in which a mold 100 including a pattern 121 according to an embodiment of the present invention is prepared.

As described above, in order to manufacture the column 1 for gas chromatography according to an embodiment of the present invention, a step S100 of preparing the mold 100 including the pattern 121 must be performed.

At this time, in one embodiment of the present invention, the mold 100 including the pattern 121 can be prepared through the step (S110) of preparing the mold 100 using a negative photoresist, as shown in FIG. 5. there is.

More specifically, through the step (S111) of forming the PR layer 120 by spin-coating a negative photoresist on the second substrate 110, the second substrate 110 is formed as shown in FIGS. 5(a) and 5(b). A PR layer 120 may be coated on the substrate 110. Thereafter, the PR layer 120 is placed on the PR layer 120 as shown in FIG. 5(c) through a step (S112) of placing a mask 130 including a through hole 131 corresponding to the shape of the pattern. ) A mask 130 including a through hole is placed on the mask 130, and a portion 121 of the PR layer is cured by irradiating ultraviolet rays toward the mask 130 (S113), as shown in FIG. 5(d). In Figure 5(e), a portion 121 of the PR layer is cured by irradiating ultraviolet rays toward the mask 130, and the other portion 122 of the PR layer is removed using a developer (S114). By removing the other part 122 of the PR layer that has not been cured by ultraviolet rays, the mold 100 including the pattern 121 according to an embodiment of the present invention as shown in FIG. 5(f) You can prepare.

4 and 5, in one embodiment of the present invention, the mold 100 including the pattern 121 can be prepared through the step (S110) of preparing the mold 100 using a negative photoresist. there is.

Figure 6 schematically shows detailed steps of preparing a mold 100 including a pattern 121 according to another embodiment of the present invention.

The detailed steps of preparing the mold 100 including the pattern 121 shown in FIG. 6 correspond to another embodiment of the step (S110) of preparing the mold 100 using a negative photoresist.

Preferably, the step (S100) of preparing the mold 100 including the pattern 121 according to another embodiment of the present invention involves irradiating plasma toward the pattern 121 to form a surface of the pattern 121. It may further include a plasma etching step (S115).

Step S115 shown in FIG. 6 corresponds to plasma etching the surface of the pattern 121 corresponding to a portion 121 of the PR layer. In step S115, after performing steps S111 to S114 described above in FIGS. 4 and 5, plasma is applied to the pattern 121 to plasma-etch the surface of the pattern 121 to increase the surface area of the pattern 121. You can do it. In one embodiment of the present invention, in the step (S115) of plasma etching the surface of the pattern 121 by irradiating plasma toward the pattern 121, O ₂ plasma may be irradiated toward the pattern 121.

When forming the upper structure 300 using the mold 100 including the pattern 121 with an increased surface area, the inner surface of the micro passage 320 formed in the upper structure 300 is the pattern 121. is formed along the surface, so that the surface area of the inner surface of the micro-channel 320 can be increased correspondingly to the surface area of the pattern 121. In particular, the upper structure 300 formed using a mold 100 including a pattern 121 whose surface area is increased through plasma etching uses a mold 100 including a pattern 121 that has not been plasma etched. Thus, a micro-passage 320 having a relatively large inner surface area compared to the upper structure 300 formed can be formed. An increase in the surface area of the inner surface of the micro-passage 320 means that the area where the sample passing through the micro-passage 320 can react increases.

That is, by increasing the surface area of the inner surface of the upper structure 300 using the mold 100 including the pattern 121 whose surface area is increased by plasma etching, the sample separation capacity of the column 1 for gas chromatography is increased. It can have the effect of increasing .

Figure 7 schematically shows an example in which a mold 100 including a pattern 121 according to another embodiment of the present invention is prepared.

As described above, in order to prepare the mold 100 including the pattern 121 according to another embodiment of the present invention, the step of plasma etching the surface of the pattern 121 corresponding to a portion 121 of the PR layer. (S115); must be further performed. At this time, step S115 can be performed by applying plasma to the second substrate 110 on which the pattern 121 is formed, as shown in FIG. 7(a).

In addition, when performing step S115, plasma is applied while the second substrate 110 on which the pattern 121 is formed is tilted at a preset angle, as shown in FIGS. 7(b) and 7(c). It may be possible. Plasma can be applied not only to the top surface but also to the side surfaces of the pattern 121, so that the surface of the pattern 121 can be plasma-etched more homogeneously.

Preferably, in the step (S115) of plasma etching the surface of the pattern 121 by irradiating plasma toward the pattern 121 according to an embodiment of the present invention, the plane on which the second substrate 110 is disposed is The upper, left, and right sides of the pattern 121 can be plasma etched by applying plasma to the pattern 121 while rotating the second substrate 110 at a preset angle about a parallel axis. .

Figure 8 schematically shows detailed steps of preparing a mold 100 including a pattern 121 according to another embodiment of the present invention.

The detailed steps of preparing the mold 100 including the pattern 121 shown in FIG. 8 correspond to the step (S120) of preparing the mold 100 using a 3D printer.

In the step of preparing the mold 100 using the 3D printer (S120), the mold 100 including the pattern 121 can be prepared by forming the pattern 121 on the substrate using the 3D printer.

Preferably, the step of preparing the mold 100 including the pattern 121 according to another embodiment of the present invention (S100) includes forming the third substrate 140 by 3D printing (S121); and forming the pattern 121 on the third substrate 140 by 3D printing (S122).

Step S121 shown in FIG. 8 corresponds to forming the third substrate 140 by 3D printing. In step S121, the third substrate 140 corresponding to the base portion of the mold 100 can be formed by 3D printing.

Step S122 shown in FIG. 8 corresponds to forming the pattern 121 on the third substrate 140 by 3D printing. In step S122, the pattern 121 can be formed by 3D printing on the third substrate 140 formed in step S121.

The pattern 121 preferably includes one of a spiral type and a parallel stacked type.

Figure 9 schematically shows an example in which a mold 100 including a pattern 121 according to another embodiment of the present invention is prepared.

As described above, in order to manufacture the column 1 for gas chromatography according to an embodiment of the present invention, a step S100 of preparing the mold 100 including the pattern 121 must be performed.

At this time, in another embodiment of the present invention, the mold 100 including the pattern 121 can be prepared through the step (S120) of preparing the mold 100 using a 3D printer, as shown in FIG. 9. .

More specifically, the third substrate 140 corresponding to the base portion of the mold 100 is formed as shown in FIG. 9(a) through the step (S121) of forming the third substrate 140 by 3D printing. can do. Afterwards, through the step (S122) of 3D printing the pattern 121 on the third substrate 140, the pattern 121 is 3D printed on the third substrate 140 as shown in FIG. 9(b). By doing so, the mold 100 including the pattern 121 according to another embodiment of the present invention can be prepared.

In this way, the mold 100 according to an embodiment of the present invention can be prepared through one of the embodiments of FIGS. 4 to 5, 4 to 7, and 8 to 9 described above.

Figure 10 conceptually shows an example of coating the stationary phase material 321 on the inner surface of the micro-passage 320 according to an embodiment of the present invention.

The gas chromatography column 1 according to an embodiment of the present invention has a micro passage 320 inside the inner surface of the upper structure 300 and a portion of the upper surface of the first substrate 400. may be formed, and the inner surface of the micro-passage 320 may be coated with a stationary phase material 321.

As described above, the upper structure 300 of the column 1 for gas chromatography may itself be formed of the stationary phase material 321. A plurality of pores 311 may be formed on the inside of the upper structure 300 due to material characteristics or plasma etching of the surface of the pattern 121. Some of the plurality of pores 311 may be excessively formed and the upper structure 300 may be formed excessively. If the pores 311 of the inner surface of the structure 300 are very large, the separation performance may actually deteriorate.

Considering this, the present invention fills the inside of the micro-passage 320 by injecting the stationary phase material 321 into the micro-passage 320 as shown in FIG. 10 and then suctioning the micro-passage 320 again. ), the separation performance of the gas chromatography column (1) was improved by coating the stationary phase material (321) on the inner surface of the column (1).

More specifically, in one embodiment of the present invention, the stationary phase material 321 is injected into the inside of the micro-passage 320 as shown in FIG. 10(a) to form the micro-passage 320 as shown in FIG. 10(b). By filling the interior of the micro-passage 320 and applying suction force to the inside of the micro-passage 320 to remove part of the stationary phase material 321 injected into the micro-passage 320, the micro-passage (321) is removed as shown in Figure 10(c). A stationary phase material 321 may be coated on the inner surface of 320).

The stationary phase material 321 coated on the inner surface of the micro-passage 320 is preferably in a liquid state. The stationary phase material 321 according to an embodiment of the present invention may include an ionic liquid. That is, the stationary phase material 321 coated on the inner surface of the micro-passage 320 corresponds to a different material from the stationary phase material (polydimethylsiloxane (PDMS)) forming the upper structure 300.

That is, in the present invention, in order to improve the separation performance of the column 1 for gas chromatography, a stationary bed containing an ionic liquid is placed on the inner side of the superstructure 300 made of a stationary bed material containing polydimethylsiloxane (PDMS). The material 321 can be coated.

In this way, when the stationary phase material 321 is additionally coated on the inner surface of the micro-passage 320 formed in the upper structure 300, the pores 311 formed relatively deeply in the micro-passage 320 can be blocked, which can be used for gas chromatography. This can have the effect of improving the separation performance of the column (1).

Figure 11 schematically shows a cross section of the superstructure 300 and the pores 311 formed in the superstructure 300 according to an embodiment of the present invention.

Figures 11(a) to 11(c) schematically show a cross section of the upper structure 300. The upper side of the upper structure 300 shown in FIGS. 11(a) to 11(c) corresponds to the micro passage 320 formed in the upper structure 300, and the lower side of the upper structure 300 is It corresponds to the outside of the upper structure 300.

As shown in FIG. 11(a), a plurality of pores 311 having different depths may be formed inside the upper structure 300. As described above, if the porosity 311 is very large due to the plurality of pores 311, the separation performance of the gas chromatography column 1 may be adversely affected, and as shown in FIG. 11(b), the upper structure A stationary phase material 321 containing an ionic liquid may be coated on the inner surface of the micro-channel 320 formed in 300 .

Additionally, as shown in FIG. 11(c), after forming the buffer layer 322 on the inner surface of the micro-channel 320, a stationary phase material 321 containing an ionic liquid may be coated on the buffer layer 322. Preferably, the micro-passage 320 according to an embodiment of the present invention has a buffer layer 322 formed on the inner surface, and the buffer layer 322 may be coated with a stationary phase material 321 on the upper surface. In one embodiment of the present invention, the buffer layer 322 may include polytetrafluoroethylene (PTFE).

In this way, by coating the inner surface of the micro-passage 320 with the buffer material 322 before coating the stationary phase material 321, the pore treatment effect by the stationary phase material 321 can be improved.

Figure 12 schematically shows an embodiment of the superstructure 300 according to an embodiment of the present invention.

In one embodiment of the present invention, the shape of the upper structure 300 formed by curing the curable polymer material 200 may vary depending on the amount of the curable polymer material 200 injected into the mold 100. Depending on the environment, part of the superstructure 300 may be removed.

Figure 12(a) shows the upper structure 300 formed by injecting and curing the curable polymer material 200 in a state where the curable polymer material 200 is injected into the mold 100 in an amount greater than the preset amount. A cross section is schematically shown. In this case, an unnecessary area A may be formed on the lower side of the micro-passage 320 as shown in FIG. 12(a), and the area A may be removed as shown in FIG. 12(b).

Figure 13 schematically shows an embodiment of the superstructure 300 according to an embodiment of the present invention.

In one embodiment of the present invention, before injecting the curable polymer material 200 for forming the superstructure 300 into the mold 100, the mold 100 is preferably placed inside the open chamber 2. do. At this time, the shape of the upper structure 300 formed by curing the curable polymer material 200 may vary depending on the position of the mold 100 within the open chamber 2, and the upper structure 300 may vary depending on the working environment. Part of the structure 300 may be removed.

Figure 13(a) shows the upper structure formed by injecting and curing the curable polymer material 200 with the mold 100 disposed at a distance B from the inner side of the open chamber 2 ( 300) schematically shows a cross section. In this case, an unnecessary area B may be formed on the lower side of the micro-passage 320 as shown in FIG. 13(a), and the area B may be removed as shown in FIG. 13(b).

Figure 14 schematically shows an embodiment of the superstructure 300 according to an embodiment of the present invention.

In one embodiment of the present invention, the upper structure 300 is formed by curing the curable polymer material 200 according to the position of the pattern 121 formed on the second substrate 110 constituting the mold 100. The shape may be variable, and a portion of the upper structure 300 may be removed depending on the working environment.

FIG. 14(a) schematically shows a cross-section of the upper structure 300 formed by injecting and curing the curable polymer material 200 with the pattern 121 formed only at the center of the second substrate 110. do. In this case, an unnecessary area C may be formed on the lower side of the micro-passage 320 as shown in FIG. 14(a), and the area C may be removed as shown in FIG. 14(b).

Meanwhile, in one embodiment of the present invention, a gas chromatography system including a column 1 for gas chromatography can be provided.

Preferably, in the gas chromatography system including the column 1 for gas chromatography according to an embodiment of the present invention, the column 1 for gas chromatography is a mold including a pattern 121 ( 100) preparing; Injecting a curable polymer material 200 into the mold 100 including the pattern 121 and curing it; removing the cured curable polymer material (200) from the mold (100) to form a superstructure (300); And placing a first substrate 400 on the lower surface of the upper structure 300, and bonding the upper structure 300 and the first substrate 400 to each other to form the gas chromatography column 1. It is manufactured through a step; and a micro-passage 320 having a height of 300 micrometers or less may be formed therein.

In addition, in one embodiment of the present invention, a method of manufacturing a gas chromatography system including the column 1 for gas chromatography can also be provided.

Preferably, a method of manufacturing a gas chromatography system including a column 1 for gas chromatography according to an embodiment of the present invention includes the steps of preparing a mold 100 including a pattern 121; Injecting a curable polymer material 200 into the mold 100 including the pattern 121 and curing it; removing the cured curable polymer material (200) from the mold (100) to form a superstructure (300); And placing a first substrate 400 on the lower surface of the upper structure 300, and bonding the upper structure 300 and the first substrate 400 to each other to form the gas chromatography column 1. step; and the gas chromatography column 1 may have a micro-passage 320 formed therein with a height of 300 micrometers or less.

As such, the present invention is a column for gas chromatography that does not require a process for forming a stationary bed material because the column itself is made of a stationary bed material, and the column can be mass-produced more easily by using the mold 100 when manufacturing the column. In addition to providing (1), a method for manufacturing the same, a gas chromatography system including the same, and a method for manufacturing the gas chromatography system can be provided.

According to one embodiment of the present invention, since the superstructure is formed with a curable polymer material, which is a type of stationary phase material, a separate process for forming the stationary phase material on the inner surface of the micro-channel is not required, thereby improving manufacturability. It can be effective.

According to an embodiment of the present invention, a superstructure is formed using a mold containing a pattern and bonded to a substrate to form a column, thereby enabling the mass production of multiple columns more easily and increasing productivity. can be demonstrated.

According to one embodiment of the present invention, when a stationary phase material is additionally coated on the inner surface of the micro-passage formed in the superstructure, pores formed relatively deeply in the micro-passage can be blocked, thereby improving the separation performance of the gas chromatography column. It can be effective.

According to one embodiment of the present invention, the effect of improving the pore treatment effect by the stationary phase material can be achieved by coating the inner surface of the micro-channel with a buffer material before coating the stationary phase material.

According to one embodiment of the present invention, the sample separation capacity of the gas chromatography column can be increased by increasing the surface area of the inner surface of the superstructure using a mold including a pattern with an increased surface area by plasma etching. can be demonstrated.

As described above, although the embodiments have been described with limited examples and drawings, various modifications and variations can be made by those skilled in the art from the above description. For example, the described techniques are performed in a different order than the described method, and/or components of the described system, structure, device, circuit, etc. are combined or combined in a different form than the described method, or other components are used. Alternatively, appropriate results may be achieved even if replaced or substituted by an equivalent. Therefore, other implementations, other embodiments, and equivalents of the claims also fall within the scope of the claims described below.

1: Column for gas chromatography
100: mold
110: second substrate 120: PR layer
121: Part of the PR layer (pattern) 122: Another part of the PR layer
130: Mask 131: Through hole corresponding to the shape of the pattern
140: Third substrate 200: Curable polymer material
300: superstructure
310: channel groove 311: pore
320: microchannel 321: stationary phase material
322: buffer layer
400: First substrate 2: Open chamber

Claims (16)

A method of manufacturing a column for gas chromatography,
Preparing a mold containing a pattern;
Injecting a curable polymer material into a mold containing the pattern and curing it;
removing the cured curable polymer material from the mold to form a superstructure; and
A step of placing a first substrate on the lower surface of the upper structure and bonding the upper structure and the first substrate to each other to form the gas chromatography column,
A method of manufacturing a column for gas chromatography, wherein the column for gas chromatography has a micro-passage with a height of 300 micrometers or less formed therein.
In claim 1,
A method of manufacturing a column for gas chromatography, wherein the curable polymer material includes polydimethylsiloxane (PDMS).
In claim 1,
The step of preparing a mold containing the pattern is,
Forming a PR layer by spin coating a negative photoresist on a second substrate;
disposing a mask including through holes corresponding to the shape of the pattern on the PR layer;
curing a portion of the PR layer by irradiating ultraviolet rays toward the mask; and
Removing another part of the PR layer using a developer,
A method of manufacturing a column for gas chromatography, wherein a portion of the PR layer corresponds to the pattern.
In claim 1,
The step of preparing a mold containing the pattern is,
Forming a third substrate by 3D printing; and
A method of manufacturing a column for gas chromatography, comprising: forming the pattern by 3D printing on the third substrate.
In claim 1,
The column for gas chromatography is,
A micro-passage may be formed within the inner surface of the upper structure and a portion of the upper surface of the first substrate,
A method of manufacturing a column for gas chromatography, wherein the micro-passage is coated with a stationary phase material on the inner surface.
In claim 1,
The column for gas chromatography is,
A micro-passage may be formed within the inner surface of the upper structure and a portion of the upper surface of the first substrate,
The micro-passage has a buffer layer formed on the inner side,
A method of manufacturing a column for gas chromatography, wherein the buffer layer is coated with a stationary phase material on the upper surface.
The method of claim 5 or 6,
A method of manufacturing a column for gas chromatography, wherein the stationary phase material includes an ionic liquid.
In claim 1,
A method of manufacturing a column for gas chromatography, wherein the pattern includes one of a spiral type and a parallel stacked type.
As a column for gas chromatography,
Preparing a mold containing a pattern; Injecting a curable polymer material into a mold containing the pattern and curing it; removing the cured curable polymer material from the mold to form a superstructure; and placing a first substrate on the lower surface of the upper structure and bonding the upper structure and the first substrate to form the column for gas chromatography,
The column for gas chromatography is a column for gas chromatography in which a micro-passage having a height of 300 micrometers or less is formed therein.
In claim 9,
A column for gas chromatography, wherein the curable polymer material includes polydimethylsiloxane (PDMS).
In claim 9,
The column for gas chromatography is,
A micro-passage may be formed within the inner surface of the upper structure and a portion of the upper surface of the first substrate,
A column for gas chromatography, wherein the micropassage is coated with a stationary phase material on the inner surface.
A gas chromatography system including a column for gas chromatography,
The column for gas chromatography is,
Preparing a mold containing a pattern; Injecting a curable polymer material into a mold containing the pattern and curing it; removing the cured curable polymer material from the mold to form a superstructure; and placing a first substrate on the lower surface of the upper structure and bonding the upper structure and the first substrate to form the gas chromatography column.
A gas chromatography system including a column for gas chromatography, inside which a micro-passage with a height of 300 micrometers or less is formed.
In claim 12,
A gas chromatography system comprising a column for gas chromatography, wherein the curable polymer material includes polydimethylsiloxane (PDMS).
In claim 12,
The column for gas chromatography is,
A micro-passage may be formed within the inner surface of the upper structure and a portion of the upper surface of the first substrate,
A gas chromatography system including a column for gas chromatography, wherein the micro-passage is coated with a stationary phase material on its inner surface.
A method of manufacturing a gas chromatography system including a column for gas chromatography,
Preparing a mold containing a pattern;
Injecting a curable polymer material into a mold containing the pattern and curing it;
removing the cured curable polymer material from the mold to form a superstructure; and
A step of placing a first substrate on the lower surface of the upper structure and bonding the upper structure and the first substrate to each other to form the gas chromatography column,
A method of manufacturing a gas chromatography system including a column for gas chromatography, wherein the column for gas chromatography has a micro-passage with a height of 300 micrometers or less formed therein.
In claim 15,
A method of manufacturing a gas chromatography system including a column for gas chromatography, wherein the curable polymer material includes polydimethylsiloxane (PDMS).

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