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Micro gas chromatographic column chip with high aspect ratio and preparation method thereof

A micro gas chromatography and high aspect ratio technology, which is used in the field of separation of mixed gases and the preparation of high aspect ratio micro gas chromatography columns, can solve the problems of difficulty in increasing the aspect ratio of the channel, uneven heating on one side, and achieve the thermal expansion coefficient. Consistent, enhanced separation and resolution, strong bonding results

Active Publication Date: 2017-05-31
XI AN JIAOTONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is to solve the problem that the aspect ratio of the channel formed by silicon-glass bonding of silicon-based micro-chromatographic column is difficult to increase, and the heating on one side is uneven. A preparation method for a chromatographic column chip, which can double the aspect ratio of the channel on the basis of the original etching. At the same time, there are heating wires and temperature measuring resistors on the front and back, so that the inside of the channel is heated more uniformly, further improving Improving the Separation Power of Microcolumns

Method used

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  • Micro gas chromatographic column chip with high aspect ratio and preparation method thereof
  • Micro gas chromatographic column chip with high aspect ratio and preparation method thereof
  • Micro gas chromatographic column chip with high aspect ratio and preparation method thereof

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preparation example Construction

[0035] image 3 (a)-(e) are process flow charts of the method for preparing a high aspect ratio micro gas chromatographic column chip according to an embodiment of the present invention. Include the following steps:

[0036] 1) Design and manufacture mask plate: according to figure 1 , 2 The structure of the design shown, fabricated on a glass substrate figure 1 , 2 (a)-(b) shows a continuous serpentine channel, in which circular columns are arranged in an array, and the spacing of the columns is symmetrically and unequally spaced.

[0037] 2) Silicon wafer pretreatment: clean the silicon wafer, place the silicon wafer in a mixed solution of concentrated sulfuric acid and hydrogen peroxide solution heated at 100-120°C in a volume ratio of 3:1, and clean it for 5-8 minutes. Rinse well and blow dry with air, then dry the silicon.

[0038] 3) Photolithography: choose a polished silicon wafer with a thickness of 500 μm as the silicon substrate, and then spin-coat photoresist...

Embodiment 1

[0046] Place the silicon wafer in a solution heated at 120°C, concentrated sulfuric acid and hydrogen peroxide solution at a volume ratio of 3:1, wash for 5 minutes, rinse with deionized water, dry with air, and then bake at 90°C Dry the silicon wafer for 10 minutes. Spin-coat photoresist N244 on the silicon wafer, place the silicon wafer with spin-coated photoresist on a heating plate at 95° C. for 5 minutes, and dry it.

[0047] Place the dried silicon wafer on the photolithography table, align the mask plate and stick it to the silicon wafer, set the exposure time to 6s, and immediately place the exposed silicon wafer on a heating plate at 120°C for intermediate baking. The time is 3 minutes, and then the silicon wafer is placed in 2.5% tetramethylammonium hydroxide solution for development, and the development time is 30s. After development, it can be seen that the pattern of the mask plate has been transferred to the silicon wafer. Dry the wafer for 10 min.

[0048] A m...

Embodiment 2

[0052] Place the silicon wafer in a solution heated at 100°C, concentrated sulfuric acid and hydrogen peroxide solution at a volume ratio of 3:1 and wash for 8 minutes, rinse with deionized water, dry with air, and then bake at 85°C Dry the silicon wafer for 10 minutes. Spin-coat photoresist N244 on the silicon wafer, place the silicon wafer with spin-coated photoresist on a heating plate at 85° C. for 8 minutes, and dry it.

[0053] Place the dried silicon wafer on the photolithography table, align the mask plate and stick it to the silicon wafer, set the exposure time for 5s, and immediately place the exposed silicon wafer on a heating plate at 110°C for intermediate baking. The time is 5 minutes, and then the silicon wafer is placed in a 2.5% tetramethylammonium hydroxide solution for development, and the development time is 25 seconds. After development, it can be seen that the pattern of the mask plate has been transferred to the silicon wafer. Dry the wafer for 15 minut...

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Abstract

The invention discloses a preparation method of a micro gas chromatographic column chip with a high aspect ratio. The method comprises the steps of manufacturing a metal pattern plate, preprocessing a silicon wafer, performing a uniform adhesive photolithography technology, and performing developing; then, sputtering a metal aluminum layer to be adopted as a masking layer, performing ultrasonic stripping, enabling a channel to be etched to be exposed, performing deep dry etching, and adjusting perpendicular etching and sedimentation protection parameters; performing anodic bonding on two substrates with identical etching graphs, sputtering a thin film heater and a temperature measuring resistor on the two faces of the substrates obtained after bonding is completed; forming a PDMS thin film inside a micro chromatographic column by adopting a static coating method. According to the obtained micro gas chromatographic column, the side wall is steep, the aspect ratio is large, the aspect ratio of the micro gas chromatographic column is increased by one time on the basis of original etching, the preparation method is simple and reliable, and the obtained micro gas chromatographic column chip is high in sensitivity and resolution ratio.

Description

technical field [0001] The invention relates to the technical field of chromatographic analysis, belongs to the field of miniaturization of chromatographic instruments, and in particular relates to a preparation method of a high-aspect-ratio micro gas chromatographic column, which can be used for separating mixed gases. Background technique [0002] Gas chromatography is a chemical analysis technique used to separate and detect the components of a gas mixture. When the mixed gas passes through the chromatographic column, due to the difference in physical or chemical properties of different components, the force between them and the stationary phase will be different, resulting in the separation of the mixed gas components and flowing out from the end of the chromatographic column at different times. The traditional gas chromatograph is mainly composed of carrier gas, sampler, chromatographic column and detector. The core component of the chromatographic column is generally a...

Claims

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Application Information

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IPC IPC(8): G01N30/60
CPCG01N30/6052G01N30/6095
Inventor 王海容吴桂珊李长青黄浩段滨韩宝庆王久洪
Owner XI AN JIAOTONG UNIV
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