集成实现功能硅微机气相色谱系统的基本元件的设计与制造

E. Kolesar, R. Reston
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引用次数: 1

摘要

利用现代硅微加工技术和VLSI电路加工技术,设计、制造和开发了微型气相色谱(GC)系统。气相色谱系统由微型进样器组成,进样器包含一个10 μ1的样品回路;一个长0.9 m(宽300 μm,高10 μm)的矩形毛细管柱,涂有0.2 μm厚的酞菁铜(CuPc)固定相;以及基于纸杯涂层化学电阻器和市售125 μm直径热导率检测器(TCD)珠的双探测器方案。采用硅微加工技术制作进样器与气相色谱柱、气相色谱柱本身和双检测器腔之间的界面。开发了一种新的集成电路薄膜加工技术,将CuPc固定相涂层涂在气相色谱系统的柱壁上,这些柱壁上微机械加工在主硅片衬底和Pyrex®盖板上,然后静电粘合在一起。采用传统的VLSI电路加工技术,设计和制作了纸杯涂层化学电阻器。该微型气相色谱系统已经证明了在等温操作(55-80°C)时直接完全分离百万分之一(ppm)氨和二氧化氮浓度的能力。在氦气载气和氮气稀释剂的作用下,在40 psi下注入10 μl含氨和二氧化氮的样品,在不到30分钟的时间内就可以分离出来。
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Design and Fabrication of the Fundamental Components Integrated to Realize a Functional Silicon Micromachined Gas Chromatography System
A miniature gas chromatography (GC) system has been designed, fabricated and developed using modem silicon micromachining and VLSI circuit processing techniques. The GC system is composed of a miniature sample injector that incorporates a 10 μ1 sample loop; a 0.9 m long, rectangular-shaped (300 μm width and 10 μm height) capillary column coated with a 0.2 μm thick copper phthalocyanine (CuPc) stationary phase; and a dual-detector scheme based upon a CuPc-coated chemiresistor and a commercially available, 125-μm diameter thermal conductivity detector (TCD) bead. Silicon micromachining was employed to fabricate the interface between the sample injector and the GC system’s column, the GC system’s column itself, and the dual-detector cavity. A novel integrated circuit thin film processing technique was developed to sublime the CuPc stationary phase coating on the GC system’s column walls micromachined in the host silicon wafer substrate and the Pyrex® cover plate which are subsequently electrostatically bonded together. The CuPc-coated chemiresistor was designed and fabricated using conventional VLSI circuit processing techniques. The miniature GC system has demonstrated the capability to directly and completely separate parts-per-million (ppm) ammonia and nitrogen dioxide concentrations when isothermally operated (55–80°C). With a helium carrier gas and nitrogen diluent, a 10 μl sample volume containing ammonia and nitrogen dioxide injected at 40 psi can be separated in less than 30 minutes.
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