Matthew W. Moorman

A monolithically-integrated μGC chemical sensor system.

Gas chromatography (GC) is used for organic and inorganic gas detection with a range of applications including screening for chemical warfare agents (CWA), breath analysis for diagnostics or law enforcement purposes, and air pollutants/indoor air quality monitoring of homes and commercial buildings. A field-portable, light weight, low power, rapid response, micro-gas chromatography (μGC) system is essential for such applications. We describe the design, fabrication and packaging of μGC on monolithically-integrated Si dies, comprised of a preconcentrator (PC), μGC column, detector and coatings for each of these components. An important feature of our system is that the same mechanical micro resonator design is used for the PC and detector. We demonstrate system performance by detecting four different CWA simulants within 2 min. We present theoretical analyses for cost/power comparisons of monolithic versus hybrid μGC systems. We discuss thermal isolation in monolithic systems to improve overall performance. Our monolithically-integrated μGC, relative to its hybrid cousin, will afford equal or slightly lower cost, a footprint that is 1/2 to 1/3 the size and an improved resolution of 4 to 25%.

Mass-Sensitive Microfabricated Chemical Preconcentrator

This paper describes a mass-sensitive microfabricated preconcentrator for use in chemical detection microsystems. The device combines mass sensing and preconcentration to create a smart preconcentrator (SPC) that determines when it has collected sufficient analyte for analysis by a downstream chemical microsystem. The SPC is constructed from a Lorentz-force-actuated pivot-plate resonator with an integrated heater. Subsequent to microfabrication, the SPC is coated with an adsorbent for collection of chemical analytes. The frequency of operation varies inversely with the mass of collected analyte. Such shifts can be measured by a back-EMF in the SPCs drive/transducer line. By using a calibrated vapor system, the limit of detection of the SPC was determined to be less than 50 ppb for dimethyl-methyl-phosphonate (DMMP) (actual limits of detection are omitted due to export control limitations). At 1 ppm of DMMP, 1-s collection was sufficient to trigger analysis in a downstream microsystem; other micropreconcentrators would require an arbitrary collection time, normally set at 1 min or longer. This paper describes the theory of operation, design, fabrication, coating, vapor system testing, and integration of the SPC into microanalytical systems. The theory of operation, which is applicable to other torsional oscillators, is used to predict a shear modulus of silicon (100) of G = 57.0 GPa plusmn2.2 GPa.

Microcombustor array and micro-flame ionization detector for hydrocarbon detection

This paper describes results from using a microcombustor to create two hydrocarbon gas sensors: one utilizing calorimetry and the other a flame ionization detector (FID) mechanism. The microcombustor consists of a catalytic film deposited on the surface of a microhotplate. This micromachined design has low heat capacity and thermal conductivity, making it ideal for heating catalysts placed on its surface. The catalytic materials provide a natural surface-based method for flame ignition and stabilization and are deposited using a micropen system, which allows precise and repeatable placement of the materials. The catalytic nature of the microcombustor design expands the limits of flammability (LoF) as compared with conventional diffusion flames; an unoptimized LoF of 1-32% for natural gas in air was demonstrated with the microcombustor, whereas conventionally 4-16% is observed. The LoF for hydrogen, methane, propane and ethane are likewise expanded. Expanded LoF permit the use of this technology in applications needing reduced temperatures, lean fuel/air mixes, or low gas flows. By coupling electrodes and an electrometer circuit with the microcombustor, the first ever demonstration of a microFID utilizing premixed fuel and a catalytically-stabilized flame has been performed; the detection of 1.2-2.9 % of ethane in a hydrogen/air mix is shown.

Micro-Flame Ionization Detection Using a Catalytic Micro-combuster

A microflame-based detector has been developed for sensing a broad range of chemical analytes. This detector combines calorimetry and flame ionization detection (FID) to produce unique analyte signatures. The microcombustor consists of a micromachined microhotplate with a catalyst on its surface, such as platinum/alumina, to rapidly initiate the ionization event. The low power microcombustor design permits quick, efficient heating of the deposited film. To perform calorimetric detection of analytes, the change in power required to maintain the resistive microhotplate heater at a constant temperature is measured. For FID, electrodes are placed around the microcombustor flame zone with an electrometer circuit measuring the production of ions. The calorimetric and FID modes respond generally to all hydrocarbons. Importantly these detection modes can be established on one convenient simultaneous microcombustor platform. The performance of the microFID mode is emphasized herein

Isothermal mass flow measurements in microfabricated rectangular channels over a very wide Knudsen range

Measurement and modeling of gas flows in microelectromechanical systems (MEMS) scale channels are relevant to the fundamentals of rarefied gas dynamics (RGD) and the practical design of MEMS-based flow systems and micropumps. We describe techniques for building robust, leak-free, rectangular microchannels which are relevant to micro- and nanofluidic devices, while the channels themselves are useful for fundamental RGD studies. For the first time, we report the isothermal steady flow of helium (He) gas through these channels from the continuum to the free-molecular regime in the unprecedented Knudsen range of 0.03–1000. On the high end, our value is 20-fold larger than values previously reported by Ewart et al (2007 J. Fluid Mech. 584 337–56). We accomplished this through a dual-tank accumulation technique which enabled the monitoring of very low flow rates, below 10−14 kg s−1. The devices were prebaked under vacuum for 24 h at 100 °C in order to reduce outgassing and attain high Kn. We devised fabrication methods for controlled-depth micro-gap channels using silicon for both channel ceiling and floor, thereby allowing direct comparisons to models which utilize this simplifying assumption. We evaluated the results against a closed-form expression that accurately reproduces the continuum, slip, transition, and free-molecular regimes developed partly by using the direct simulation Monte Carlo method. The observed data were in good agreement with the expression. For Kn > ~100, we observed minor deviations between modeled and experimental flow values. Our fabrication processes and experimental data are useful to fundamental RGD studies and future MEMS microflow devices with respect to extremely low-flow measurements, model validation, and predicting optimal designs.

Micro-analytical systems for national security applications

Sandia National Laboratories has a long tradition of technology development for national security applications. In recent years, significant effort has been focused on micro-analytical systems - handheld, miniature, or portable instruments built around microfabricated components. Many of these systems include microsensor concepts and target detection and analysis of chemical and biological agents. The ultimate development goal for these instruments is to produce fully integrated sensored microsystems. Described here are a few new components and systems being explored: (1) A new microcalibrator chip, consisting of a thermally labile solid matrix on an array of suspended-membrane microhotplates, that when actuated delivers controlled quantities of chemical vapors. (2) New chemical vapor detectors, based on a suspended-membrane micro-hotplate design, which are amenable to array configurations. (3) Micron-scale cylindrical ion traps, fabricated using a molded tungsten process, which form the critical elements for a micro-mass analyzer. (4) Monolithically integrated micro-chemical analysis systems fabricated in silicon that incorporate chemical preconcentrators, gas chromatography columns, detector arrays, and MEMS valves.

Invited article: A materials investigation of a phase-change micro-valve for greenhouse gas collection and other potential applications.

The deleterious consequences of climate change are well documented. Future climate treaties might mandate greenhouse gas (GHG) emissions measurement from signatories in order to verify compliance. The acquisition of atmospheric chemistry would benefit from low cost, small size/weight/power of microsystems. In this paper, we investigated several key materials science aspects of a phase-change microvalve (PCμV) technology with low power/size/weight/cost for ubiquitous GHG sampling. The novel design, based on phase-change material low-melting-point eutectic metal alloys (indium-bismuth, InBi and tin-lead, SnPb), could be actuated at temperatures as low as 72 °C. Valve manufacturing was based on standard thick and thin-film processes and solder technologies that are commonly used in industry, enabling low-cost, high-volume fabrication. Aging studies showed that it was feasible to batch fabricate the PCμVs and store them for future use, especially in the case of SnPb alloys. Hermetic sealing of the valve prototypes was demonstrated through helium leak testing, and Mil spec leak rates less than 1 × 10(-9) atm cm(3)/s were achieved. This confirms that the sample capture and analysis interval can be greatly expanded, easing the logistical burdens of ubiquitous GHG monitoring. Highly conservative and hypothetical CO(2) bias due to valve actuation at altitude in 1 cm(3) microsamplers would be significantly below 1.0 and 2.2 ppmv for heat-treated InBi and SnPb solders, respectively. The CO(2) bias from the PCμV scales well, as a doubling of sampler volume halved the bias. We estimated the shelf life of the SnPb PCμVs to be at least 2.8 years. These efforts will enable the development of low cost, low dead volume, small size/weight microsystems for monitoring GHGs and volatile organic compounds.

A highly miniaturized vacuum package for a trapped ion atomic clock

We report on the development of a highly miniaturized vacuum package for use in an atomic clock utilizing trapped ytterbium-171 ions. The vacuum package is approximately 1 cm(3) in size and contains a linear quadrupole RF Paul ion trap, miniature neutral Yb sources, and a non-evaporable getter pump. We describe the fabrication process for making the Yb sources and assembling the vacuum package. To prepare the vacuum package for ion trapping, it was evacuated, baked at a high temperature, and then back filled with a helium buffer gas. Once appropriate vacuum conditions were achieved in the package, it was sealed with a copper pinch-off and was subsequently pumped only by the non-evaporable getter. We demonstrated ion trapping in this vacuum package and the operation of an atomic clock, stabilizing a local oscillator to the 12.6 GHz hyperfine transition of (171)Y b(+). The fractional frequency stability of the clock was measured to be 2 × 10(-11)/τ(1/2).

Lower heating value sensor for fuel monitoring

This work details the development of a low cost, lower heating value (LHV) sensor that consists of a catalytic film deposited on the surface of a micromachined hotplate. The micromachined sensor has low heat capacity and thermal conductivity, making it appropriate for accurate LHV determination. Catalytically combusting the fuel provides the capability of direct LHV measurement, unlike most LHV measurement systems which rely on inference. The results of extensive laboratory testing and preliminary field testing will be reported, which demonstrate the capability to measure LHV values to within +/- 5% accuracy across a wide range of fuel values. Field testing results have shown LHV determination to within +/- 1.2% over a more narrow range of fuel heating values

Development of a Mesoscale Pulsed Discharge Helium Ionization Detector for Portable Gas Chromatography

Miniaturization of gas chromatography (GC) instrumentation enables field detection of volatile organic compounds (VOCs) for chembio-applications such as clandestine human transport and disease diagnostics. We fabricated a mesoscale pulsed discharge helium ionization detector (micro-PDHID) for integrating with our previously described mini-GC hardware. Stainless steel electrodes fabricated by photochemical etching and electroforming facilitated rapid prototyping and enabled nesting of inter-electrode insulators for self-alignment of the detector core during assembly. The prototype was ∼10 cm(3) relative to >400 cm(3) of a commercial PDHID, but with a comparable time to sweep a VOC peak from the detector cell (170 ms and 127 ms, respectively). Electron trajectory modeling, gas flow rate, voltage bias, and GC outlet location were optimized for improving sensitivity. Despite 40-fold miniaturization, the micro-PDHID detected 18 ng of the human emanation, 3-methyl-2-hexenoic acid with <3-fold decrease in sensitivity relative to the commercial detector. The micro-PDHID was rugged and operated for 9 months without failure.