Publications

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We describe for the first time hydrogen bonded acid (HBA) polymer, poly[methyl[3-(2-hydroxyl, 4,6-bistrifluoromethyl)- phenyl]propylsiloxane], (DKAP), as stationary phase for gas chromatography (μGC) of organophosphate (OP), chemical warfare agent (CWA) surrogates, dimethylmethylphosphonate (DMMP), diisopropylmethylphosphonate (DIMP), diethylmethylphosphonate (DEMP), and trimethylphosphate (TMP), with high selectivity. Absorption of OPs to DKAP was one-to-several orders of magnitude higher relative to commercial polar, mid-polar, and nonpolar stationary phases. We also present for the first-time thermodynamic studies on the absorption of OP vapors and quantitative binding energy data for interactions with various stationary phases. These data help to identify the best pair of hetero-polar columns for a two-dimensional GC system, employing a nonpolar stationary phase as GC1 and DKAP as the GC2 stationary phase, for selective and rapid field detection of CWAs.

The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

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We have developed a significantly improved composite material for applications to chemiresistors, which are resistance-based sensors for volatile organic compounds. This material is a polymer composite containing Au-coated magnetic particles organized into electrically conducting pathways by magnetic fields. This improved material overcomes the various problems inherent to conventional carbon-black chemiresistors, while achieving an unprecedented magnitude of response. When exposed to chemical vapors, the polymer swells only slightly, yet this is amplified into large, reversible resistance changes - as much as 9 decades at a swelling of only 1.5 %. These conductor-insulator transitions occur over such a narrow range of analyte vapor concentration that these devices can be described as chemical switches. We demonstrate that the sensitivity and response range of these sensors can be tailored over a wide range by controlling the stress within the composite, including through the application of a magnetic field. Such tailorable sensors can be used to create sensor arrays that can accurately determine analyte concentration over a broad concentration range, or can be used to create logic circuits that signal a particular chemical environment. It is shown through combined mass-sorption and conductance measurements, that the response curve of any individual sensor is a function of polymer swelling alone. This has the important implication that individual sensor calibration requires testing with only a single analyte. In addition, we demonstrate a method for analyte discrimination based on sensor response kinetics, which is independent of analyte concentration. This method allows for discrimination even between chemically similar analytes. Lastly, additional variables associated with the composite and their effects on sensor response are explored.

We investigate the magnetostriction of field-structured magnetoelastomers, which are an important class of materials that have great potential as both sensors and actuators. Field-structured magnetoelastomers are synthesized by suspending magnetic particles in a polymeric resin and subjecting these to magnetic structuring fields during polymerization. These structuring fields can consist of as many as three orthogonal ac components, allowing a wide variety of particles structures-chains, sheets, or networks-to be formed. A principal issue is how particle structure and loading affects the magnetostriction of these materials. To investigate magnetostriction in these field-structured composites we have constructed a constant stress, optical cantilever apparatus capable of 1 ppm strain resolution. Magnetoelastomers having a wide range of particle loadings and structures are investigated, and it is shown that the observed deformation depends strongly on composite structure. The best magnetoelastomers exhibit a contractive strain of 10 000 ppm, the worst materials exhibit a negative, tensile response, which we show is due to the dominance of demagnetizing field effects over magnetostriction. Finally, some discussion is given to the surprising finding that magnetostriction is proportional to the sample prestrain. Simulations of a chain of particles in an elastomer show that particle clumping transitions can occur, but this does not account for the dependence of magnetostriction on prestrain. © 2006 The American Physical Society.

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As electronic and optical components reach the micro- and nanoscales, efficient assembly and packaging require the use of adhesive bonds. This work focuses on resolving several fundamental issues in the transition from macro- to micro- to nanobonding. A primary issue is that, as bondline thicknesses decrease, knowledge of the stability and dewetting dynamics of thin adhesive films is important to obtain robust, void-free adhesive bonds. While researchers have studied dewetting dynamics of thin films of model, non-polar polymers, little experimental work has been done regarding dewetting dynamics of thin adhesive films, which exhibit much more complex behaviors. In this work, the areas of dispensing small volumes of viscous materials, capillary fluid flow, surface energetics, and wetting have all been investigated. By resolving these adhesive-bonding issues, we are allowing significantly smaller devices to be designed and fabricated. Simultaneously, we are increasing the manufacturability and reliability of these devices.