Design and Analysis of a Preconcentrator for the ChemLab

Preconcentration is a critical analytical procedure when designing a microsystem for trace chemical detection, because it can purify a sample mixture and boost the small analyte concentration to a much higher level allowing a better analysis. This paper describes the development of a micro-fabricated planar preconcentrator for the {mu}ChemLab{trademark} at Sandia. To guide the design, an analytical model to predict the analyte transport, adsorption and resorption process in the preconcentrator has been developed. Experiments have also been conducted to analyze the adsorption and resorption process and to validate the model. This combined effort of modeling, simulation, and testing has led us to build a reliable, efficient preconcentrator with good performance

Selective, pulsed CVD of platinum on microfilament gas sensors

A post-processing, selective micro-chemical vapor deposition (``micro-CVD``) technology for the deposition of catalytic films on surface-micromachined, nitride-passivated polysilicon filaments has been investigated. Atmospheric pressure deposition of Pt on microfilaments was accomplished by thermal decomposition of Pt acetylacetonate; deposition occurs selectively only on those filaments which are electrically heated. Catalyst morphology, characterized by SEM, can be controlled by altering deposition time, filament temperature, and through the use of pulsed heating of the filament during deposition. Morphology plays an important role in determining the sensitivity of these devices when used as combustible gas sensors

Design and Testing of a Micro Thermal Conductivity Detector (TCD) System

This work describes the design, simulation, fabrication and characterization of a microfabricated thermal conductivity detector to be used as an extension of the {micro}ChemLab{trademark}. The device geometry was optimized by simulating the heat transfer in the device, utilizing a boundary element algorithm. In particular it is shown that within microfabrication constraints, a micro-TCD optimized for sensitivity can be readily calculated. Two flow patterns were proposed and were subsequently fabricated into nine-promising geometries. The microfabricated detector consists of a slender metal film, supported by a suspended thin dielectric film over a pyramidal or trapezoidal silicon channel. It was demonstrated that the perpendicular flow, where the gas directly impinges on the membrane, creates a device that is 3 times more sensitive than the parallel flow, where the gas passed over the membrane. This resulted in validation of the functionality of a microfabricated TCD as a trace-level detector, utilizing low power. the detector shows a consistent linear response to concentration and they are easily able to detect 100-ppm levels of CO in He. Comparison of noise levels for this analysis indicates that sub part per million (ppm) levels are achievable with the selection of the right set of conditions for the detector to operate under. This detector was originally proposed as part of a high-speed detection system for the petrochemical gas industry. This system was to be utilized as a process monitor to detect reactor ''upset'' conditions before a run away condition could occur (faster than current full-scale monitoring systems were able to achieve). Further outlining of requirements indicated that the detection levels likely achievable with a TCD detector would not be sufficient to meet the process condition needs. Therefore the designed and fabricated detector was integrated into a detection system to showcase some technologies that could further the development of components for the current gas phase {micro}ChemLab as well as future modifications for process monitoring work such as: pressurized connections, gas sampling procedures, and packed columns. Component integration of a microfabricated planar pre-concentrator, gas-chromatograph column and TCD in the separation/detection of hydrocarbons, such as benzene, toluene and xylene (BTX) was also demonstrated with this system

µChemLab: twenty years of developing CBRNE detection systems with low false alarm rates

Gas Chromatography (GC) is routinely used in the laboratory to temporally separate chemical mixtures into their constituent components for improved chemical identification. This paper will provide a overview of more than twenty years of development of one-dimensional field-portable micro GC systems, highlighting key experimental results that illustrate how a reduction in false alarm rate (FAR) is achieved in real-world environments. Significantly, we will also present recent results on a micro two-dimensional GC (micro GCxGC) technology. This ultra-small system consists of microfabricated columns, NanoElectroMechanical System (NEMS) cantilever resonators for detection, and a valve-based stop-flow modulator. The separation of a 29-component polar mixture in less than 7 seconds is demonstrated along with peak widths in the second dimension ranging from 10-60 ms. For this system, a peak capacity of just over 300 was calculated for separation in about 6 s. This work has important implications for field detection, to drastically reduce FAR and significantly improve chemical selectivity and identification. This separation performance was demonstrated with the NEMS resonator and bench scale FID. But other detectors, suitably fast and sensitive can work as well. Recent research has shown that the identification power of GCxGC-FID can match that of GC-MS. This result indicates a path to improved size, weight, power, and performance in micro GCxGC systems outfitted with relatively non-specific, lightweight detectors. We will briefly discuss the performance of possible options, such as the pulsed discharge helium ionization detector (PDHID) and miniature correlation ion mobility spectrometer (mini-CIMS)

Genomics-enabled sensor platform for rapid detection of viruses related to disease outbreak.

Bioweapons and emerging infectious diseases pose growing threats to our national security. Both natural disease outbreak and outbreaks due to a bioterrorist attack are a challenge to detect, taking days after the outbreak to identify since most outbreaks are only recognized through reportable diseases by health departments and reports of unusual diseases by clinicians. In recent decades, arthropod-borne viruses (arboviruses) have emerged as some of the most significant threats to human health. They emerge, often unexpectedly, from cryptic transmission foci causing localized outbreaks that can rapidly spread to multiple continents due to increased human travel and trade. Currently, diagnosis of acute infections requires amplification of viral nucleic acids, which can be costly, highly specific, technically challenging and time consuming. No diagnostic devices suitable for use at the bedside or in an outbreak setting currently exist. The original goals of this project were to 1) develop two highly sensitive and specific diagnostic assays for detecting RNA from a wide range of arboviruses; one based on an electrochemical approach and the other a fluorescent based assay and 2) develop prototype microfluidic diagnostic platforms for preclinical and field testing that utilize the assays developed in goal 1. We generated and characterized suitable primers for West Nile Virus RNA detection. Both optical and electrochemical transduction technologies were developed for DNA-RNA hybridization detection and were implemented in microfluidic diagnostic sensing platforms that were developed in this project

A MEMS Based Hybrid Preconcentrator/Chemiresistor Chemical Sensor

A hybrid of a microfabricated planar preconcentrator and a four element chemiresistor array chip has been fabricated and the performance as a chemical sensor system has been demonstrated. The close proximity of the chemiresistor sensor to the preconcentrator absorbent layer allows for fast transfer of the preconcentrated molecules during the heating and resorption step. The hybrid can be used in a conventional flow sampling system for detection of low concentrations of analyte molecules or in a pumpless/valveless mode with a grooved lid to confine the desorption plume from the preconcentrator during heating

Microfabrication of membrane-based devices by HARSE and combined HARSE/wet etching

Deep-reactive ion etching (DRIE) of silicon, also known as high-aspect-ratio silicon etching (HARSE), is distinguished by fast etch rates ({approximately}3 {micro}m/min), crystal orientation independence, anisotropy, vertical sidewall profiles and CMOS compatibility. By using through-wafer HARSE and stopping on a dielectric film placed on the opposite side of the wafer, freestanding dielectric membranes were produced. Dielectric membrane-based sensors and actuators fabricated in this way include microhotplates, flow sensors, valves and magnetically-actuated flexural plate wave (FPW) devices. Unfortunately, low-stress silicon nitride, a common membrane material, has an appreciable DRI etch rate. To overcome this problem HARSE can be followed by a brief wet chemical etch. This approach has been demonstrated using KOH or HF/Nitric/Acetic etchants, both of which have significantly smaller etch rates on silicon nitride than does DRIE. Composite membranes consisting of silicon dioxide and silicon nitride layers are also under evaluation due to the higher DRIE selectivity to silicon dioxide

Microfabrication of membrane-based devices by deep-reactive ion etching (DRIE) of silicon

Deep reactive ion etching (DRIE) of silicon was utilized to fabricate dielectric membrane-based devices such as microhotplates, valves and flexural plate wave (FPW) devices. Through-wafer DRIE is characterized by fast etch rates ({approximately} 3 {micro}m/min), crystal orientation independence, vertical sidewall profiles and CMOS compatibility. Low-stress silicon nitride, a popular membrane material, has an appreciable DRIE etch rate. To overcome this limitations DRIE can be accompanied by a brief wet chemical etch. This approach has been demonstrated using KOH or HF/Nitric/Acetic etchants, both of which have significantly lower etch rates on silicon nitride than does DRIE. The DRIE etch properties of composite membranes consisting of silicon dioxide and silicon nitride layers are also under evaluation due to the higher DRIE selectivity to silicon dioxide