Sensing of the volatile organic compounds (VOCs) isopropyl alcohol (IPA) and heptane in air using sub-millimeter porous silicon-based sensor elements is demonstrated in the concentration range 50-800 ppm. The sensor elements are prepared as one-dimensional photonic crystals (rugate fi lters) by programmed electrochemical etch of p + + silicon, and analyte sensing is achieved by measurement of the wavelength shift of the photonic resonance. The sensors are studied as a function of surface chemistry: ozone oxidation, thermal oxidation, hydrosilylation (1-dodecene), electrochemical methylation, reaction with dicholorodimethylsilane and thermal carbonization with acetylene. The thermally oxidized and the dichlorodimethylsilane-modifi ed materials show the greatest stability under atmospheric conditions. Optical microsensors are prepared by attachment of the porous Si layer to the distal end of optical fi bers. The acetylated porous Si microsensor displays a greater response to heptane than to IPA, whereas the other chemical modifi cations display a greater response to IPA than to heptane. The thermal oxide sensor displays a strong response to water vapor, while the acetylated material shows a relatively weak response. The results suggest that a combination of optical fi ber sensors with different surface chemistries can be used to classify VOC analytes. Application of the miniature sensors to the detection of VOC breakthrough in a full-scale activated carbon respirator cartridge simulator is demonstrated.
An electrochemically fabricated 1D photonic crystal of porous Si displaying a single reflectance peak is coupled to an optical fiber and embedded in activated carbon to sense the breakthrough of organic vapors (see figure). The sensor responds to various organic vapors, demonstrating filter end‐of‐ service‐life applications
The condensation and evaporation of vapors of isopropanol, heptane, and cyclohexane in mesoporous silica photonic crystals are monitored by optical reflection spectroscopy as a function of sensor temperature. The spectral position of the stop band shifts to the red upon analyte adsorption, and it shifts to the blue as the sensor is heated and analyte evaporates from the porous nanostructure. The hysteresis of the optical response as the temperature of the sensor is cycled between 25 and 80 °C is characteristic of each analyte for partial pressures between 0 and 7.5 Torr. These characteristic hysteresis loops allow identification of the three analytes. The temporal response of the sensor is studied as a function of heating rate and analyte concentration in a flowing stream of analyte vapor, and it is compared with the equilibrium adsorption isotherms of the sensor. The ability of the temporal data to identify the analytes is attributed to differences in diffusion and adsorption properties of each analyte within the mesoporous silica sensor.
We report a thermally tunable multispectral imaging filter based on reversible condensation of volatile organic fluids within a nanoporous one-dimensional photonic crystal. The photonic crystal (optical rugate filter) comprises oxidized porous silicon, prepared by electrochemical etch of silicon and subsequent air oxidation (porous silica rugate filter, pSiF). The reflectance spectrum of the pSiF is designed and constructed to match two of the red emission bands of the luminescent complex europium(III) tris-dipicolinate, [Eu(dpa)3](3-), which has been used as an indicator for anthrax spores. When the pSiF is fitted with a thermoelectric Peltier cooler/heater and sealed in a container with 2-propanol vapor, microcapillary effects drive the temperature-dependent condensation/evaporation of 2-propanol into/out of the porous nanostructure. Thermal cycling experiments show that the wavelengths of the spectral bands of the pSiF are reversibly tuned by ±35 nm for a temperature change of ±40 °C. Difference images of a UV-illuminated scene containing the [Eu(dpa)3](3-) target, obtained by reflection from pSiF that is continuously thermally cycled through the emission bands of the dye, show that the target can be discriminated from the background or from control targets with overlapping but dissimilar luminescence spectra.
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