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Forschungsbericht 2011 / Hochschule für Angewandte Wissenschaften - Fachhochschule Regensburg
(2011)
This work gives a detailed characterization of a laboratory setup for photoacoustic NO2 trace gas detection at the ppb level. The signal generation is based on the excitation of electronic 2B2 and 2B1 states using a low-cost semiconductor laser emitting at 450 nm. An acoustic resonator was used for signal amplification and the modulation frequency of the laser was determined to 3395 Hz in order to gain maximum signal amplification. The quality of resonant amplification was determined to 7.9. The gas samples were NO2 calibration gases diluted with pure nitrogen. The signal-to-noise ratio (SNR) dependency on the flow rate Q and the lock-in time constant τLIA was investigated, respectively, and the optimum values were specified to Q = 500 mL/min and τLIA = 2 s. In case of ambient noise, increasing τLIA to 10 s was evaluated as sufficient for SNR preservation. The noise level was measured in the absence of NO2 and it was determined to be composed of 51% electronic noise and 49% gas flow noise. With the analyte concentration ranging from 300 ppbV to 100 ppmV, the linear dependency of the photoacoustic amplitude on the NO2 concentration was specified, the sensitivity was determined to 110 μV/ppmV and the maximum measurement error was calculated to ±0.8%. The detection limit was determined to 2.0 ppbV. Furthermore, the stability of the signal was investigated and a maximum drift of ±1% was observed within a measuring period of 30 min. The response time τ90 was specified to 58 s. All results considered, this photoacoustic measuring system, which is based on low-cost signal generation and detection units, provides an excellent basis in view of developing a portable device for photoacoustic trace gas detection.
Diese Abhandlung beschreibt das Konzept eines mikroeletromechanischen Systems (MEMS), das im Messverfahren der cantilever enhanced photoacoustic spectroscopy (CEPAS) Verwendung finden soll.
Es wird die Herstellung eines einseitig eingespannten Biegebalkens aus Silizium mittels deep reactiv ion etching (DRIE) beschrieben. Des Weiteren wird die Resonanzfrequenz dieses Cantilevers mit Hilfe Laservibrometertechnik untersucht. Die resultierenden resonanten Schwingungen 0.Ordnung werden mit den Ergebnissen einer vereinfachten theoretischen Näherung verglichen. Die Messergebnisse stehen in gutem Zusammenhang mit den theoretischen Werten. Solche Cantilever, die aus silicon on insula tor (SOI) Wafer angefertigt wurden, weisen bei einer Zielfrequenz ein mittlere Abweichung von Δf = 118±26Hz (bzw.Δf =0,76±0,17%) auf.
We present the development and characterization as well as comprehensive interference studies of a photoacoustic NO2 trace gas detection system. The system is based on an off-beam quartz enhanced photoacoustic scheme (off-beam QEPAS) and signal generation was initiated by amplitude modulating a low-cost diode laser emitting at 450 nm. The QEPAS sensor element features double-resonant amplification, still it is only ∼ 5 × 5 × 2.5 mm in size. The individual and combined resonance characteristics were investigated and specified to 52 dB amplification, adding up 15 dB acoustic- and 37 dB mechanical-resonance amplification. The linearity of the photoacoustic signal dependency on the analyte concentration was verified from 200 ppbV to 100 ppmV NO2 in synthetic air. The detection limit (3σ) was determined to 1.8 ppbV using a lock-in time constant of 10 s and an averaging time of 20 s. The normalized noise equivalent absorption coefficient was specified to 2.5·10−8 W cm−1 Hz−0.5. The stability of the signal was investigated over time and a slight drift by 1‰ was observed after 30 min without temperature stabilizing the photoacoustic cell (PAC). Noise analysis was performed by means of Allan deviation and the inverse dependency of response time and precision of the system on the lock-in time constant was outlined. We performed interference analyses towards N2, O2, CO2, H2O and acoustic noise, respectively. Although neither spectral interferences nor losses due to slow NO2 VT-relaxation were observed, O2 was identified to cause a 15% signal drop due to VVNO2-O2-relaxation. Changing H2O concentrations were found to cause acoustic detuning, which cannot be compensated by adjusting the frequency of modulation, because of the double-resonant feature of the PAC. However, alternative approaches of compensation were discussed. Finally, we carried out heavy traffic noise simulations and determined the QEPAS setup to be 46 times less susceptible towards ambient noise compared to standard microphone-based photoacoustic setups.
Photoacoustic spectroscopy is an efficient method to detect the concentration of trace gases with following advantages: short response time, high sensitivity, continuous and real-time monitoring and the option of miniaturization without the need of complex mirror-based multi-pass cell designs. A micromechanical cantilever is used as a key component in a two-part "Cantilever-Resonator" system that detects the weak photoacoustic signal. The resonance frequency of cantilever needs to be tuned to match the resonance frequency of resonator in order to achieve the maximum vibration amplitude of the "Cantilever-Resonator" system. This paper reports a post-fabrication method to tune the resonance frequency of cantilevers via focused ion beam (FIB) and a capacitive solution for the cantilever to transform the acoustic signal to electrical signal.