CN117741029A - Micro chromatographic column with homogeneous stationary phase and its prepn process - Google Patents
Micro chromatographic column with homogeneous stationary phase and its prepn process Download PDFInfo
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- CN117741029A CN117741029A CN202311369857.6A CN202311369857A CN117741029A CN 117741029 A CN117741029 A CN 117741029A CN 202311369857 A CN202311369857 A CN 202311369857A CN 117741029 A CN117741029 A CN 117741029A
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- 230000005526 G1 to G0 transition Effects 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims description 38
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 116
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 116
- 239000000758 substrate Substances 0.000 claims abstract description 75
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 12
- 229910001887 tin oxide Inorganic materials 0.000 claims description 12
- 239000011787 zinc oxide Substances 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 11
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- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 claims description 5
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Abstract
The invention provides a micro chromatographic column with uniform stationary phase and a preparation method thereof, wherein good bonding of the substrate and a cover plate can be realized through a first hydrophilic metal oxide layer and a second hydrophilic metal oxide layer; the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer can enable the inner surface of the closed micro-channel to be homogenous, and uniformity of the hydrophilic stationary phase layer is improved; the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer can provide hydrophilic surfaces, improve the hydrophilicity of the inner surface material for closing the micro-channels, and effectively improve the uniformity of the hydrophilic stationary phase layer, thereby improving the separation performance of the micro-chromatographic column.
Description
Technical Field
The invention belongs to the field of micro-electromechanical systems, and relates to a micro-chromatographic column with a uniform stationary phase and a preparation method thereof.
Background
As a common analysis means, gas chromatography has been widely used in the fields of petrochemical industry, drug detection, energy exploration, environmental monitoring, and the like.
The core component of the gas chromatograph is a gas chromatographic column, and the gas chromatographic column is used for separating mixed sample gas to be analyzed. In the whole test system, the gas chromatographic column plays a role in separating mixed gas, and the performance of the gas chromatographic column directly influences the analysis effect of the whole gas chromatographic system. The stationary phase is one of key factors for determining the separation effect of the gas chromatographic column, and the adsorption and desorption capacities of different gases are different, so that different gas components have different flow rates in a channel, and finally, the separation of mixed gas is realized, and the problems of low separation degree, serious tailing of chromatographic peaks and the like are caused by uneven distribution of the stationary phase. Therefore, whether the stationary phase is distributed uniformly determines the quality of the separation performance, and the uniform distribution of the stationary phase is important for realizing the high-efficiency separation of the detected gas.
At present, the stationary phase forming method of the micro chromatographic column mainly comprises a dynamic coating method and a static coating method, and in addition, chemical vapor deposition, metal evaporation technology, sputtering technology and layer-by-layer stacking technology are also used in the stationary phase preparation technology, but the micro chromatographic column with uniform stationary phase is still difficult to prepare. The main reasons are two: firstly, the current micro chromatographic column is generally formed by bonding silica glass, wherein a micro channel of the micro chromatographic column is formed by two heterogeneous materials of silicon and glass, and stationary phases with uniform thickness distribution are difficult to obtain on the surfaces of the different materials; secondly, the acting force between the surface of the microchannel and the stationary phase material is weak, the stationary phase with uniform thickness distribution is difficult to obtain, and the column loss is easy to generate.
Therefore, it is necessary to provide a micro chromatographic column with uniform stationary phase and a preparation method thereof.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a micro-chromatographic column with a homogeneous stationary phase and a method for preparing the same, which are used for solving the problem of homogeneity of the stationary phase of the micro-chromatographic column in the prior art.
To achieve the above and other related objects, the present invention provides a micro-chromatography column having a uniform stationary phase, the micro-chromatography column comprising:
a substrate and a cover plate;
a microchannel located in the substrate, the microchannel having a first port and a second port;
a first hydrophilic metal oxide layer and a second hydrophilic metal oxide layer, wherein the first hydrophilic metal oxide layer covers the surfaces of the substrate and the micro-channel, the second hydrophilic metal oxide layer covers the surface of the cover plate, and the cover plate is bonded on the substrate based on the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer so as to cover the micro-channel to form a closed micro-channel;
a hydrophilic stationary phase layer covering the inner surface of the closed microchannel.
Optionally, the micro-channel comprises a micro-column array formed by combining a plurality of micro-columns, wherein the micro-columns comprise elliptical micro-columns or circular micro-columns; the micro-channel comprises a serpentine extension, a fold line extension, a U-shaped extension or a spiral extension.
Optionally, the first hydrophilic metal oxide layer includes one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer, and a hydrophilic tin oxide layer; the second hydrophilic metal oxide layer comprises one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer.
Optionally, the hydrophilic stationary phase layer comprises one or a combination of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer.
Optionally, the substrate comprises a silicon substrate, a glass substrate, or a ceramic substrate; the cover plate comprises a glass cover plate, a silicon cover plate or a ceramic cover plate.
The invention also provides a preparation method of the micro chromatographic column with the uniform stationary phase, which comprises the following steps:
providing a substrate;
patterning the substrate to form a microchannel in the substrate, the microchannel having a first port and a second port;
forming a first hydrophilic metal oxide layer covering the surface of the substrate and the microchannel;
providing a cover plate, and forming a second hydrophilic metal oxide layer on the surface of the cover plate;
bonding the cover plate to the substrate based on the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer to cover the micro-channels to form closed micro-channels;
a hydrophilic stationary phase layer is formed that covers the inner surface of the closed microchannel.
Optionally, patterning the substrate further comprises forming a micro-column array formed by combining a plurality of micro-columns in the micro-channel, wherein the micro-columns comprise elliptical micro-columns or circular micro-columns; the micro-channel is formed in a shape including a serpentine extension, a fold line extension, a U-shaped extension or a spiral extension.
Optionally, the method for forming the first hydrophilic metal oxide layer includes an ALD method, a sputtering method or an evaporation method, and the formed first hydrophilic metal oxide layer includes one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer; the method for forming the second hydrophilic metal oxide layer comprises an ALD method, a sputtering method or an evaporation method, and the formed second hydrophilic metal oxide layer comprises one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer.
Optionally, the method of forming the hydrophilic stationary phase layer comprises a coating method, and the hydrophilic stationary phase layer formed comprises one or a combination of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer.
Optionally, the method of bonding the cap plate to the substrate based on the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer includes anodic bonding.
As described above, the micro chromatographic column with uniform stationary phase and the preparation method thereof can realize good bonding of the substrate and the cover plate by the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer; the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer can enable the inner surface of the closed micro-channel to be homogenous, and uniformity of the hydrophilic stationary phase layer is improved; the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer can provide hydrophilic surfaces, improve the hydrophilicity of the inner surface material for closing the micro-channels, and effectively improve the uniformity of the hydrophilic stationary phase layer, thereby improving the separation performance of the micro-chromatographic column.
Drawings
FIG. 1 shows a flow chart of a process for preparing a micro-chromatography column in an embodiment of the invention.
FIG. 2 is a schematic diagram of a patterned substrate after forming a microchannel and a micropillar array according to an embodiment of the invention.
Fig. 3 is a schematic structural diagram of the first hydrophilic metal oxide layer formed according to an embodiment of the present invention.
Fig. 4 is a schematic structural diagram of the cover plate bonded to the substrate according to the embodiment of the invention.
FIG. 5 is a schematic diagram showing the structure of a hydrophilic stationary phase layer formed according to an embodiment of the present invention.
Fig. 6 is a schematic diagram showing the combination of a hydrophilic metal oxide layer and a hydrophilic stationary phase layer in an embodiment of the present invention.
Description of element reference numerals
100. Substrate and method for manufacturing the same
101. Micro-column array
102. Micro-channel
103. First port
104. Second port
201. First hydrophilic metal oxide layer
202. Second hydrophilic metal oxide layer
300. Cover plate
400. Closed microchannel
500. Hydrophilic stationary phase layer
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
As described in detail in the embodiments of the present invention, the cross-sectional view of the device structure is not partially enlarged to a general scale for convenience of explanation, and the schematic drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in actual fabrication.
For ease of description, spatially relative terms such as "under", "below", "beneath", "above", "upper" and the like may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that these spatially relative terms are intended to encompass other orientations of the device in use or operation in addition to the orientation depicted in the figures, including embodiments in which the first and second features are formed in direct contact, as well as embodiments in which additional features are formed between the first and second features, such that the first and second features may not be in direct contact, and further, when a layer is referred to as being "between" two layers, it may be the only layer between the two layers, or there may be one or more intervening layers.
It should be noted that, the illustrations provided in the present embodiment merely illustrate the basic concept of the present invention by way of illustration, and only the components related to the present invention are shown in the drawings and are not drawn according to the number, shape and size of the components in actual implementation, and the form, number and proportion of each component in actual implementation may be changed at will, and the layout of the components may be more complex.
Referring to fig. 2 to 5, the present embodiment provides a micro chromatographic column having a uniform stationary phase, the micro chromatographic column comprising:
a substrate 100 and a cover plate 300;
a microchannel 102, the microchannel 102 being located in the substrate 100, the microchannel 102 having a first port 103 and a second port 104;
a micro-pillar array 101, the micro-pillar array 101 being located in the micro-channel 102;
a first hydrophilic metal oxide layer 201 and a second hydrophilic metal oxide layer 202, wherein the first hydrophilic metal oxide layer 201 covers the surfaces of the substrate 100, the micro-channel 102 and the micro-pillar array 101, the second hydrophilic metal oxide layer 202 covers the surface of the cover plate 300, and the cover plate 300 is bonded on the substrate 100 based on the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 to cover the micro-channel 102 to form a closed micro-channel 400, such that the hydrophilic metal oxide layer is attached to the surface of the closed micro-channel 400;
hydrophilic stationary phase layer 500, said hydrophilic stationary phase layer 500 covering the inner surface of said closed micro-channel 400.
In the present embodiment, the micro-channel 102 is provided with the micro-column array 101 formed by combining a plurality of micro-columns, but the present invention is not limited thereto, and in another embodiment, the micro-channel 102 may not be provided with the micro-column array 101, and may be specifically selected according to need.
Specifically, in the microchromatography column of the present embodiment, by covering the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 on the surfaces of the substrate 100, the microchannel 102 and the micropillar array 101, when the substrate 100 and the cover 300 in the microchromatography column are made of different materials and the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 are made of the same material, the homogeneous bonding between the substrate 100 and the cover 300 can be realized, and the bonding force can be further improved; the presence of the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 may homogenize the inner surface of the closed micro-channel 400, so that the hydrophilic stationary phase layer 500 is in contact with only the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202, and thus, the uniformity of the distribution of the hydrophilic stationary phase layer 500 may be improved.
Further, since the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 have hydrophilicity, a hydrophilic surface can be provided to improve the hydrophilicity of the inner surface material of the closed micro channel 400, and when contacting the hydrophilic stationary phase layer 500 having hydrophilicity, the uniformity of the distribution of the hydrophilic stationary phase layer 500 can be effectively improved, thereby improving the separation performance of the micro chromatographic column.
As an example, the first hydrophilic metal oxide layer 201 may include one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer, and a hydrophilic tin oxide layer; the second hydrophilic metal oxide layer 202 may comprise one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer, and a hydrophilic tin oxide layer.
Specifically, the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 can provide hydrophilic groups so as to combine with the hydrophilic stationary phase layer 500 having hydrophilic groups, so that the acting force of the interface is improved, the hydrophilic stationary phase layer 500 is uniformly distributed, and column loss is not easy to occur.
The first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 may be made of the same material, but of course, may be made of different materials according to the needs, and the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 may be a single layer or a laminated composite structure, which is not limited herein and may be selected according to the needs.
In this embodiment, the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 are preferably made of homogeneous materials, and the hydrophilic aluminum oxide layer is selected as the hydrophilic metal oxide layer, but not limited thereto, and the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 may also be laminated composite structures according to needs, wherein the hydrophilic metal oxide layer exposed on the surface layer of the closed micro-channel 400 is preferably made of homogeneous materials, so as to improve the bonding binding force between the hydrophilic metal oxide layer and the hydrophilic stationary phase layer 500.
As an example, the hydrophilic stationary phase layer 500 may include one or a combination of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer, but is not limited thereto.
Specifically, the adsorption and desorption capacities of the hydrophilic stationary phase layer 500 on different gases are different, so that the flow rates of different gas components in the closed micro-channel 400 are different, and the time from the first port 103 to the second port 104 is different, so that the separation of the mixed gases can be realized.
Wherein, by the hydrophilic property of the hydrophilic stationary phase layer 500, the hydrophilic stationary phase layer 500 has a good acting force with the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 on the inner surface of the closed micro channel 400, so as to improve the distribution uniformity of the hydrophilic stationary phase layer 500.
Regarding the choice of material for the hydrophilic stationary phase layer 500, it may be a single hydrophilic MOF layer, such as HKUST-1 layer, uiO-67 layer, etc., to provide hydrophilic groups, such as-NH 2 The hydrophilic stationary phase layer 500 may be a hydrophilic mesoporous silica layer, or the hydrophilic stationary phase layer 500 may be a laminated composite structure of a hydrophilic MOF, or a laminated composite structure composed of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer, etc., as required.
In the embodiment shown in fig. 6, the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 are both hydrophilic aluminum oxide layers, and the hydrophilic stationary phase layer 500 is HKUST-1 layers to form a good bonding force, but the selection of the first hydrophilic metal oxide layer 201, the second hydrophilic metal oxide layer 202 and the hydrophilic stationary phase layer 500 is not limited thereto.
As an example, the substrate 100 may include a silicon substrate, a glass substrate, or a ceramic substrate; the cover plate 300 may comprise a glass cover plate, a silicon cover plate, or a ceramic cover plate.
Specifically, the substrate 100 and the cover 300 may be made of the same material, but may be made of different materials according to the needs, and may be specifically selected according to the needs. In this embodiment, the substrate 100 is a silicon substrate, and the cover 300 is a glass cover, but is not limited thereto.
As an example, the micropillars in the micropillar array 101 may comprise elliptical micropillars or circular micropillars.
In particular, when the micro-pillars are elliptical micro-pillars, it is preferable that the major axis direction of the elliptical micro-pillars is parallel to the extending direction of the micro-channels 102, and the minor axis direction of the elliptical micro-pillars is parallel to the width direction of the micro-channels 102, as shown in fig. 2, the micro-pillar array 101 may be formed by arranging a plurality of micro-pillars in the micro-channels 102, so that the area of the "quasi-zero flow velocity zone" formed by the micro-pillars is greatly reduced, so that the hydrophilic stationary phase layer 500 is uniformly attached, and the flow velocity distribution in the pillars is uniform, but not limited thereto, and the micro-pillars may also be circular micro-pillars, and the specific shape of the micro-pillar array 101 is not limited thereto.
By way of example, the topography of the microchannel 102 may comprise a serpentine extension, a polyline extension, a U-shaped extension, or a spiral extension.
Specifically, in the embodiment shown in fig. 2, the micro-channel 102 extends in a serpentine shape, however, in other examples, the micro-channel 102 may extend in any extending manner in the substrate 100, such as a fold line extending, a U-shaped extending, a spiral extending, etc., which is not limited herein.
Referring to fig. 1, the present invention also provides a method for preparing a micro chromatographic column with a homogeneous stationary phase, comprising the steps of:
s1: providing a substrate 100;
s2: patterning the substrate 100 to form a micro-channel 102 and a micro-pillar array 101 in the substrate 100, wherein the micro-channel 102 has a first port 103 and a second port 104, and the micro-pillar array 101 is located in the micro-channel 102;
s3: forming a first hydrophilic metal oxide layer 201 covering the substrate 100, the microchannels 102, and the surface of the micropillar array 101;
s4: providing a cover plate 300, and forming a second hydrophilic metal oxide layer 202 on the surface of the cover plate 300;
s5: bonding the cap plate 300 to the substrate 100 based on the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 to cover the microchannel 102 to form a closed microchannel 400;
s6: a hydrophilic stationary phase layer 500 is formed, and the hydrophilic stationary phase layer 500 covers the inner surface of the closed micro channel 400.
Specifically, the microcolumn may be prepared by the method, but is not limited to the method, and may be adaptively changed according to the need, in this embodiment, the microcolumn array 101 formed by combining a plurality of microcolumns in the microchannel is formed when patterning the substrate 100, but is not limited to this, and in another embodiment, the microcolumn array 101 may not be disposed in the microchannel 102, and may be specifically selected according to the need.
The preparation of the microcomprhromatography column is described below with reference to FIGS. 2 to 5.
First, referring to fig. 1 and 2, step S1 and step S2 are performed to provide a substrate 100, and patterning the substrate 100, forming a micro-channel 102 and a micro-pillar array 101 in the substrate 100, wherein the micro-channel 102 has a first port 103 and a second port 104, and the micro-pillar array 101 is located in the micro-channel 102.
Specifically, the substrate 100 may include a silicon substrate, a glass substrate, a ceramic substrate, or the like, the substrate 100 may be patterned by using a DRIE process, for example, a mask layer (not shown), such as a silicon oxide mask layer, a silicon nitride mask layer, or a photoresist mask layer, may be formed on the surface of the substrate 100, the mask layer is patterned by photolithography and etching, and then the substrate 100 is etched to form the micro-channel 102 and the micro-pillar array 101 having the first port 103 and the second port 104 in the substrate 100, and then the mask layer is removed. The method of patterning the substrate 100 is not limited to a DRIE process.
Next, referring to fig. 1 and 3, step S3 is performed to form a first hydrophilic metal oxide layer 201 covering the surfaces of the substrate 100, the micro channel 102 and the micro pillar array 101.
Wherein, the method of forming the first hydrophilic metal oxide layer 201 may include, but is not limited to, an Atomic Layer Deposition (ALD) method, a sputtering method, or an evaporation method, and the first hydrophilic metal oxide layer 201 may be formed to include one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer, and a hydrophilic tin oxide layer. In this embodiment, the atomic layer deposition method is a preferred method because of its excellent performance in conformally depositing thin films in the high aspect ratio of the microchannels 102.
Next, referring to fig. 1 and 4, step S4 is performed to provide a cover plate 300, and a second hydrophilic metal oxide layer 202 is formed on the surface of the cover plate 300.
Specifically, the cover plate 300 may include a glass cover plate, a silicon cover plate, or a ceramic cover plate, where the cover plate 300 and the substrate 100 may be made of the same material or different materials, which is not limited herein.
Wherein, the method of forming the second hydrophilic metal oxide layer 202 may include, but is not limited to, an Atomic Layer Deposition (ALD) method, a sputtering method, or an evaporation method, and the formed second hydrophilic metal oxide layer 202 may include one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer, and a hydrophilic tin oxide layer.
The method for preparing the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 is not limited herein, but is preferably ALD, and the materials of the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 may be homogeneous or heterogeneous, which is not limited herein.
Next, referring to fig. 1 and 4, step S5 is performed to bond the cover plate 300 to the substrate 100 based on the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 to cover the micro-channel 102 to form a closed micro-channel 400.
Wherein the cover plate 300 may be bonded to the substrate 100 using, but not limited to, an anodic bonding process, the bonding process conditions may be selected as desired, and are not limited thereto.
Specifically, the cover 300 may be placed on a cathode of a bonding machine, the substrate 100 may be placed on an anode of the bonding machine to perform anodic bonding of silicon glass, after bonding is completed, dicing may be performed to expose the first port 103 and the second port 104, and then fixing capillaries (not shown) may be installed on the first port 103 and the second port 104, so as to facilitate the preparation of the hydrophilic stationary phase layer 500.
In this embodiment, the first hydrophilic metal oxide layer 201 and the second hydrophilic metal oxide layer 202 are preferably made of a homogeneous material, so as to improve the bonding force between the cover plate 300 and the substrate 100, and to improve the distribution uniformity of the hydrophilic stationary phase layer 500.
Next, referring to fig. 1 and 5, step S6 is performed to form a hydrophilic stationary phase layer 500, wherein the hydrophilic stationary phase layer 500 covers the inner surface of the closed micro-channel 400.
In particular, the method of forming the hydrophilic stationary phase layer 500 may employ a coating method, such as a dynamic coating method, but is not limited thereto, and the hydrophilic stationary phase layer 500 may be formed to include one or a combination of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer.
Regarding the types and beneficial effects of the first hydrophilic metal oxide layer 201, the second hydrophilic metal oxide layer 202, and the hydrophilic stationary phase layer 500, the description thereof will be omitted herein, and the description of the micro chromatographic column can be referred to above.
In summary, according to the micro chromatographic column with the uniform stationary phase and the preparation method thereof, good bonding of the substrate and the cover plate can be realized through the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer; the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer can enable the inner surface of the closed micro-channel to be homogenous, and uniformity of the hydrophilic stationary phase layer is improved; the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer can provide hydrophilic surfaces, improve the hydrophilicity of the inner surface material for closing the micro-channels, and effectively improve the uniformity of the hydrophilic stationary phase layer, thereby improving the separation performance of the micro-chromatographic column.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. A microchromatography column having a homogeneous stationary phase, said microchromatography column comprising:
a substrate and a cover plate;
a microchannel located in the substrate, the microchannel having a first port and a second port;
a first hydrophilic metal oxide layer and a second hydrophilic metal oxide layer, wherein the first hydrophilic metal oxide layer covers the surfaces of the substrate and the micro-channel, the second hydrophilic metal oxide layer covers the surface of the cover plate, and the cover plate is bonded on the substrate based on the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer so as to cover the micro-channel to form a closed micro-channel;
a hydrophilic stationary phase layer covering the inner surface of the closed microchannel.
2. The microchromatography column of claim 1 wherein: the micro-column array is positioned in the micro-channel and consists of a plurality of micro-columns, and the micro-columns comprise elliptical micro-columns or circular micro-columns; the micro-channel comprises a serpentine extension, a fold line extension, a U-shaped extension or a spiral extension.
3. The microchromatography column of claim 1 wherein: the first hydrophilic metal oxide layer comprises one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer; the second hydrophilic metal oxide layer comprises one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer.
4. The microchromatography column of claim 1 wherein: the hydrophilic stationary phase layer comprises one or a combination of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer.
5. The microchromatography column of claim 1 wherein: the substrate comprises a silicon substrate, a glass substrate or a ceramic substrate; the cover plate comprises a glass cover plate, a silicon cover plate or a ceramic cover plate.
6. A method for preparing a microcolumn having a homogeneous stationary phase, comprising the steps of:
providing a substrate;
patterning the substrate to form a microchannel in the substrate, the microchannel having a first port and a second port;
forming a first hydrophilic metal oxide layer covering the surface of the substrate and the microchannel;
providing a cover plate, and forming a second hydrophilic metal oxide layer on the surface of the cover plate;
bonding the cover plate to the substrate based on the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer to cover the micro-channels to form closed micro-channels;
a hydrophilic stationary phase layer is formed that covers the inner surface of the closed microchannel.
7. The method of preparing a microcolumn according to claim 6, wherein: forming a micro-column array formed by combining a plurality of micro-columns in the micro-channel when patterning the substrate, wherein the micro-columns comprise elliptical micro-columns or circular micro-columns; the micro-channel is formed in a shape including a serpentine extension, a fold line extension, a U-shaped extension or a spiral extension.
8. The method of preparing a microcolumn according to claim 6, wherein: the method for forming the first hydrophilic metal oxide layer comprises an ALD method, a sputtering method or an evaporation method, and the formed first hydrophilic metal oxide layer comprises one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer; the method for forming the second hydrophilic metal oxide layer comprises an ALD method, a sputtering method or an evaporation method, and the formed second hydrophilic metal oxide layer comprises one or a combination of a hydrophilic aluminum oxide layer, a hydrophilic zinc oxide layer and a hydrophilic tin oxide layer.
9. The method of preparing a microcolumn according to claim 6, wherein: the method of forming the hydrophilic stationary phase layer comprises a coating method, and the formed hydrophilic stationary phase layer comprises one or a combination of a hydrophilic MOF layer and a hydrophilic mesoporous silica layer.
10. The method of preparing a microcolumn according to claim 6, wherein: the method of bonding the cap plate to the substrate based on the first hydrophilic metal oxide layer and the second hydrophilic metal oxide layer includes anodic bonding.
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