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A kind of micro gas chromatographic column which can use air as carrier gas and preparation method thereof

A technology of micro gas chromatography and production method, which is applied to high reliability micro gas chromatography column, separation of complex multi-component organic compound gas, and high resolution fields, and can solve the problem of poor stability, increased coating area of ​​stationary phase, and insufficient separation performance. and other problems, to achieve the effect of increasing the inner wall roughness, increasing the coating surface area, and better thermal stability

Active Publication Date: 2022-07-12
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems of insufficient separation performance, poor stability and the need for high-purity carrier gas in the current microchromatography technology, the present invention aims to invent a micro-chromatographic column with high stability and high column efficiency, which uses air as the carrier gas (no need to carry additional carrier gas cylinders) , the stationary phase support on the inner surface of the chromatographic column provides a rough surface, and its mesoporous structure greatly increases the coating area of ​​the stationary phase, improving the separation ability within the limited length of the chromatographic column

Method used

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  • A kind of micro gas chromatographic column which can use air as carrier gas and preparation method thereof
  • A kind of micro gas chromatographic column which can use air as carrier gas and preparation method thereof
  • A kind of micro gas chromatographic column which can use air as carrier gas and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0074] In step 1), photolithography is performed on an N-type double-sided polished single-sided oxidized silicon wafer 1 with a thickness of 4 inches and a thickness of 500 nm, and an aluminum mask layer 5 with a thickness of 160 nm is formed by electron beam evaporation and lift-off.

[0075] In step 2), using aluminum as a mask, a chromatographic column micro-channel 2 is formed by a deep reactive ion etching method. The dimensions of the column micro-channel are: total length 3m; width 200um; depth 250um; micro-column arrays are regularly arranged in the column micro-channel, the column cross-section is circular, the diameter is 30um, and the spacing on the flow rate section is 26um. 29um from the wall in the vertical flow direction.

[0076] Step 3), soaking and cleaning the micro-channel of the chromatographic column with a mixed solution whose mass ratio is 60°C of concentrated sulfuric acid: water: nitric acid=16:4:1 and a mixed solution whose mass ratio is concentrate...

Embodiment 2

[0096] In step 1), photolithography is performed on an N-type double-sided polished single-sided oxidized silicon wafer 1 with a thickness of 4 inches and a thickness of 600 nm, and an aluminum mask layer 5 with a thickness of 150 nm is formed by electron beam evaporation and peeling.

[0097] In step 2), using aluminum as a mask, a chromatographic column micro-channel 2 is formed by a deep reactive ion etching method. The dimensions of the chromatographic column microchannel are: total length 1m; width 200um; depth 100um; micro-column arrays are regularly arranged in the chromatographic column microchannel, the column cross section is square, the side length is 30um, and the spacing on the flow velocity section is 25um, 30um from the wall in the vertical flow direction.

[0098] Step 3), soaking and cleaning the micro-channel of the chromatographic column with a mixed solution whose mass ratio is 60°C of concentrated sulfuric acid: water: nitric acid=16:4:1 and a mixed soluti...

Embodiment 3

[0117] In step 1), photolithography is performed on an N-type double-sided polished single-sided oxidized silicon wafer 1 with a thickness of 4 inches and a thickness of 800 nm, and an aluminum mask layer 5 with a thickness of 170 nm is formed by electron beam evaporation and lift-off.

[0118] In step 2), using aluminum as a mask, a chromatographic column micro-channel 2 is formed by a deep reactive ion etching method. The dimensions of the column microchannel are: total length 3m; width 200um; depth 300um; micro-column arrays are regularly arranged in the column microchannel, the column cross section is circular, the diameter is 30um, and the spacing on the flow rate section is 25um , 30um from the wall in the vertical flow direction.

[0119] Step 3), soaking and cleaning the micro-channel of the chromatographic column with a mixed solution whose mass ratio is 60°C of concentrated sulfuric acid: water: nitric acid=16:4:1 and a mixed solution whose mass ratio is concentrated...

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Abstract

The invention discloses a micro gas chromatography column that can use air as a carrier gas and a manufacturing method thereof, which comprises the steps of forming an aluminum mask layer by photolithography peeling on a silicon wafer; ; Soak the silicon wafer in acid solution, remove the mask and bond with borosilicate glass; sputter titanium and platinum on the back of the silicon wafer as temperature measuring resistance, heating wire and electrode; sputter gold as electrode pins; capillary connection to micro gas chromatography The column has two ports; mesoporous silica microspheres are constructed in the microfluidic channel of the chromatographic column, and the ionic liquid stationary phase is coated by static coating. The mesoporous structure in the chromatographic column greatly increases the coating area of ​​the stationary phase, improves the separation ability within the limited length of the chromatographic column, has a good tolerance to oxygen, and ensures the high reliability of the micro-chromatographic column in a high-temperature aerobic environment It has high stability, high stability and high column efficiency, and can directly use air as the carrier gas, providing an excellent micro-chromatographic column for the VOCs detection system.

Description

technical field [0001] The invention relates to the technical field of chromatographic analysis and the field of micro-electronic mechanical systems, in particular to a high-resolution, high-reliability micro gas chromatographic column that can use air as a carrier gas and a manufacturing method thereof, and the invention is suitable for complex multi-component organic compound gases It can be applied to on-site respiratory diagnosis, environmental monitoring, etc. Background technique [0002] Gas chromatography is an efficient method for separating and detecting mixtures. The chromatographic columns used in traditional gas chromatography are packed columns or fused silica capillary columns, which have long column length, large volume, and long separation time. Therefore, the chromatographic system also has the problems of large volume, slow analysis, and high power consumption, which is difficult to achieve. It is applied to the analysis of field tests such as respiratory...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60B01D15/10B01D53/04B01J20/283B01J20/30
CPCG01N30/6095G01N30/606B01D15/10B01J20/283B01D53/04B01D2257/708
Inventor 王海容石路嘉王久洪吴欣雨韩宝庆王大祚陈家洛
Owner XI AN JIAOTONG UNIV
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