In the current work, a novel combustion method is demonstrated for the direct synthesis of nanocomposite materials. Specifically doped tin dioxide (SnO 2 ) powders were selected for the demonstration studies due to the key role SnO 2 plays in semiconductor gas sensors and the strong sensitivity of doped SnO 2 to nanocomposite properties. The synthesis approach combines solid and gas-phase precursors to stage the decomposition and particle nucleation processes. A range of synthesis conditions and four material systems were examined in the study: gold-tin dioxide, palladium-tin dioxide, copper-tin dioxide, and aluminum-tin dioxide. Several additive precursors were considered including four metal acetates and two pure metals. The nanocomposite materials produced were examined for morphology, phase, composition, and lattice spacing using transmission and scanning electron microscopy, x-ray diffractometry, and energy-dispersive spectroscopy. The results using the combustion synthesis approach indicate good control of the nanocomposite properties, such as the average SnO 2 crystallite size, which ranged from 5.8 to 17 nm.
High surface area, active catalysts containing dispersed catalytic platinum nanoparticles (d p ∼ 11.6 nm) on a cordierite substrate were fabricated and characterized using TEM, XRD, and SEM. The catalyst activity was evaluated for methanol oxidation. Experimental results were obtained in a miniature-scale continuous flow reactor. Subsequent studies on the effect of catalyst loading and reactor flow parameters are reported. Repeat tests were performed to assess the stability of the catalyst and the extent of deactivation, if any, that occurred due to restructuring and sintering of the particles. SEM characterization studies performed on the postreaction catalysts following repeat tests at reasonably high operating temperatures (∼500• C corresponding to ∼0.3T m for bulk platinum) showed evidence of sintering, yet the associated loss of surface area had minimal effect on the overall catalyst activity, as determined from bulk temperature measurements. The potential application of this work for improving catalytic devices including microscale reactors is also briefly discussed.
This work demonstrates the variability in performance between SnO2 thick film gas sensors prepared using two types of film deposition methods. SnO2 powders were deposited on sensor platforms with and without the use of binders. Three commonly utilized binder recipes were investigated, and a new binder-less deposition procedure was developed and characterized. The binder recipes yielded sensors with poor film uniformity and poor structural integrity, compared to the binder-less deposition method. Sensor performance at a fixed operating temperature of 330 °C for the different film deposition methods was evaluated by exposure to 500 ppm of the target gas carbon monoxide. A consequence of the poor film structure, large variability and poor signal properties were observed with the sensors fabricated using binders. Specifically, the sensors created using the binder recipes yielded sensor responses that varied widely (e.g., S = 5 – 20), often with hysteresis in the sensor signal. Repeatable and high quality performance was observed for the sensors prepared using the binder-less dispersion-drop method with good sensor response upon exposure to 500 ppm CO (S = 4.0) at an operating temperature of 330 °C, low standard deviation to the sensor response (±0.35) and no signal hysteresis.
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