Fabrication and Testing of High Aspect Ratio Metal Micro-Gas Chromatograph Columns

Bhushan, Abhinav; Yemane, Dawit; Goettert, Jost; Overton, Edward B.; Murphy, Michael C.

doi:10.1115/imece2004-62115

Cited by 11 publications

(13 citation statements)

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“…Beginning with Terry's original idea of a microfabricated GC column (Terry and Herman 1979), a number of research groups have developed micro-GC columns in silicon (Hudson et al 1998;Whiting et al 2001;Kolesar and Reston 1996), parylene (Noh et al 2002), and metal (Bhushan et al 2004a). The microfabricated silicon GC columns, typically 40 lm wide, 250 lm deep, and 1 m long, consist of a silicon substrate micromachined using the Bosch DRIE process and a cover sheet of Pyrex Ò .…”

Section: Introductionmentioning

confidence: 98%

Fabrication of micro-gas chromatograph columns for fast chromatography

et al. 2006

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Gas chromatography (GC) is one of the most widespread techniques used in laboratories as a way to separate and analyze complex mixtures of volatile and semi-volatile compounds. The main advantage of miniaturization of these systems is the increased performance due to the reduced time for analysis and reduced fabrication cost of the complex pneumatic flow system. In this paper advanced design ideas and fabrication processes to facilitate integration of the sample concentrator and the column will be presented. Using the LIGA process, 0.5-and 2-m-long, 50-lm-wide, and up to 600-lm-high aspect ratio metal GC separation columns with on-chip integrated sample injection and detection were fabricated. Initial experiments of coating these high aspect ratio columns show promising results when compared to simple tubular columns.

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Section: Introductionmentioning

confidence: 98%

Fabrication of micro-gas chromatograph columns for fast chromatography

et al. 2006

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“…The first efforts to produce a µGC began in 1970 at Stanford University [1], with more recent efforts at Lawrence Livermore [2] and Sandia National Laboratories [3]. Various column structures have been explored, including anodically-bonded glass-silicon columns [2,3,4], silicon/silicon dioxide fusion-bonded columns [5], metal LIGA-based columns [5], and parylene columns [6]. Although these efforts have yielded important progress, they have not yet provided the high performance and low-power operation needed for many applications.…”

Section: Introductionmentioning

confidence: 99%

A Low-Power Pressure- And Temperature-Programmable Micro Μgc Column

Potkay¹,

Lambertus²,

Sacks³

et al. 2006

2006 Solid-State, Actuators, and Microsystems Workshop Technical Digest

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This paper presents the theory, fabrication and experimental results for the highest performance, low-power micro gas chromatography ( GC) column realized to date. The suspendeddielectric 1m-long column is split into two sections, permitting pressure programming. Furthermore, each section is individually temperature programmable. The integrated heaters have a mean resistance of 6.8 k and a TCR of 1439 ppm/ºC. A single heater in the fully suspended column requires 6 mW to raise the local column temperature by 100 ºC in vacuum (10 µTorr). The column has separated 10 alkanes in 52 s and four chemical warfare agent simulants and an explosive simulant in 60s.

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“…Since the introduction of silicon-microchip gas-chromatography (GC) columns by Terry et al in 1979, there has been tremendous interest among researchers in fabricating such columns in various substrates such as ceramics, , glass, polymers, , and metals. ,− Despite the wide variety of substrates employed, silicon accounts for the majority, at approximately 80% of all microchip GC columns fabricated. The advantages of silicon include established micromachining technology, the capability of generating high-aspect-ratio features, cost effectiveness due to batch processing, low thermal mass, high thermal conductivity, chemical inertness, and silanol (Si–OH) chemistry similar to that of the popular fused-silica capillary column technology .…”

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“…Unsatisfied by the performance of first-generation silicon–glass hybrid systems that were mainly limited to isothermal operation because of high thermal capacitance and low thermal conductivity, Bhushan et al became the first to report the use of a metal microchip GC column in 2004. This initial report was followed by several detailed descriptions of metallic columns in later years. , These columns were fabricated by X-ray LIGA using two substrates: one sacrificial (titanium or silicon) and the other the final substrate (nickel), where the sacrificial substrate was used as an initial support that was eventually etched away, leaving the final electrodeposited substrate.…”

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confidence: 99%

“…Unsatisfied by the performance of first-generation silicon− glass hybrid systems that were mainly limited to isothermal operation because of high thermal capacitance and low thermal conductivity, Bhushan et al 7 became the first to report the use of a metal microchip GC column in 2004. This initial report was followed by several detailed descriptions of metallic columns in later years.…”

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Stainless-Steel Column for Robust, High-Temperature Microchip Gas Chromatography

et al. 2018

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13This paper reports the first results of a robust, high performance, stainless-steel 14 microchip gas chromatography (GC) column that is capable of analyzing complex real 15 world mixtures as well as operating at very high temperatures. Using a serpentine 16 design, a 10 m column with an approximately semicircular cross section with a 52 µm 17 hydraulic diameter (Dh) was produced in a 17 cm x 6.3 cm x 0.1 cm rectangular steel 18 chip. The channels were produced using a multilayer chemical etch and diffusion 19 bonding process, and metal nuts were brazed onto the inlet and outlet ports allowing for 20 column interfacing with ferrules and fused silica capillary tubing. After deactivating the 21 metal surface, channels were statically coated with a layer of 0.16 µm (5%-phenyl)(1%-22 vinyl)-methylpolysiloxane (SE-54) stationary phase, and cross-linked with dicumyl 23 peroxide. By using n-tridecane (n-C13) as test analyte with a retention factor (k) of 5, a 24 total of 44,500 plates (≈4500 plates/m) was obtained isothermally at 120 °C. The 25 column was thermally stable to at least 350 °C, and rapid temperature programming (35 26 °C/min) was demonstrated for the boiling point range from n-C5 to n-C44 (ASTM D 2887 27 simulated distillation standard). The column was also tested for separation of two 28 complex mixtures: gasoline headspace and kerosene. These initial experiments 29 demonstrate that the planar stainless-steel column with proper interfacing can be a 30 viable alternative platform for portable, robust microchip GC that is capable of high 31 temperature operation for low volatility compound analysis. Since the introduction of silicon microchip gas chromatography (GC) columns by 34 Terry et al. (1) in 1979, there has been tremendous interest among researchers in 35 fabricating such columns in various substrates such as ceramics (2,3) glass (4), 36 polymers (5, 6) and metals (2, 7-9). Despite the wide variety of substrates employed, 37 silicon accounts for the majority at approximately 80% of all microchip GC columns 38 fabricated. The advantages of silicon include established micromachining technology, 39 capability of generating high aspect ratio features, cost effectiveness due to batch 40 processing, low thermal mass, high thermal conductivity, chemical inertness and 41 familiar silanol (Si-OH) chemistry to the popular fused-silica capillary column technology 42 (10). It is worth mentioning that although there are reports of all-silicon microcolumns 43 (both etched in and bonded with silicon wafers), in most cases, the channels are 44 microfabricated in a silicon substrate followed by anodically bonding to a Pyrex glass 45 top layer (1, 11,12). This design is not ideal as such silicon/glass hybrid systems exhibit 46 thermal expansion coefficient (CTE) mismatch (13), non-uniformity in temperature 47 91 column. After bonding the channels, stainless steel connection tubes were brazed to the 92 plate for connection to the inlet and detector. Unlike epoxy-based adhesives, since 93 brazing can handle high...

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Fabrication and Testing of High Aspect Ratio Metal Micro-Gas Chromatograph Columns

Cited by 11 publications

References 0 publications

Fabrication of micro-gas chromatograph columns for fast chromatography

Fabrication of micro-gas chromatograph columns for fast chromatography

A Low-Power Pressure- And Temperature-Programmable Micro Μgc Column

Stainless-Steel Column for Robust, High-Temperature Microchip Gas Chromatography

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