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- Coulometric sensors (3)
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Organisationseinheit der BAM
A silicon MIS-structure prepared with thin layers of the super-ionic conductor LaF3 and Pd is used to detect hydrogen. The sensor is able to detect hydrogen in a concentration range from below one ppm to the lower flammable limit in air which is 4 vol.-%. The chip operates at room temperature which results in an extremely low energy consumption compared to other hydrogen sensors. Only once per day a short heating pulse is necessary to reactivate the sensor chip. In cooperation with the BAM, a long-term experiment was carried out. The duration of the measurement was about three months, with a hydrogen exposure every two weeks. The sensor signal remained stable over the measured period.
The efficiency of gas sensor application for facilitating the safe use of hydrogen depends to a considerable extent on the response time of the sensor to change in hydrogen concentration. The response and recovery times have been measured for five different hydrogen sensors, three commercially available and two promising prototypes which operate at room temperature.
Experiments according to ISO 26142 show that most of the sensors surpass much for a concentration change from clean to hydrogen containing air the demands of the Standard for the response times t(90) and values of 2 to lös were estimated. For an opposite shift to clean air, the recovery times t(10) are from 7 to 70 s. Results of transient behaviour can be fitted with an exponential approach. It can be demonstrated that results on transient behaviour depend not only from investigation method, and the experimental conditions, like gas changing rate and concentration jump, as well as from operating
Parameters of sensors. In comparison to commercial MOS and MIS-FET hydrogen sensors new sensor prototypes operating at room temperature possesses in particular longer recovery times.
Ionische Flüssigkeiten als neuartige Sensorbeschichtung für coulometrische Spurenfeuchtesensoren
(2018)
Die Arbeit präsentiert erste Messungen mit coulometrischen Sensoren, die mit einer ionischen Flüssigkeit beschichtet sind. Diese Sensoren werden in der Industrie verwendet, um die Spurenfeuchte in unterschiedlichen Gasen zu messen. Normalerweise erfolgt eine Beschichtung der Sensoren mit Phosphorpentoxid und dessen Hydrolyseprodukte. In dieser Arbeit wurde stattdessen eine hygroskopische ionische Flüssigkeit benutzt. Die generierte Gasfeuchte für die Untersuchungen betrug bezogen auf die Frostpunkttemperatur -80 °C bis -30 °C, was gleichbedeutend mit einem Wasserdampf-Stoffmengenanteil von 0,5 μmol·mol-1 bis 376 μmol·mol-1 ist. Zusätzlich zu der Messung mit coulometrischen Sensoren erfolgte eine Referenzmessung der Gasfeuchte mittels eines Taupunkthygrometers. Erste Ergebnisse haben gezeigt, dass es möglich ist mit dieser Art der Beschichtung unterschiedliche Gasfeuchten zu messen. Aber es ergaben sich trotz gleicher Feuchte unterschiedliche Signalintensitäten bei den benutzen Sensoren und es zeigte sich eine Drift des Sensorsignales.
This work presents a first attempt to use ionic liquids as a new coating for planar coulometric sensors. These sensors are used for the measurement of trace humidity in various gases. Usually, the coating of the sensors is tetraphosphorus decaoxide and its hydrolysis products. Instead, a hygroscopic ionic liquid was used as sensor coating in this work. Generated frost point temperatures tf in the gas ranged from -80 °C to -30 °C, which is equivalent to vapour mole fractions xv from 0.5 μmol·mol-1 to 376 μmol·mol-1. In addition to the coulometric sensors, the generated humidity is determined by a precision dew point hygrometer as reference. First results show that it is possible to measure humidity with ionic liquid based coulometric sensors.
Planar coulometric sensors were investigated in humidified synthetic air at various absolute gas pressures, i. e. 2 bar, 5, bar, 10 bar, and 15 bar. Humidified gas flow at adjusted gas pressure was split into two flows, one passed a coulometric sensor and the other one passed a reference hygrometer after decompression. Both signals were recorded and then compared after calculation of resulting frost point temperature. Calculation is based on a calibration function obtained at ambient pressure. Comparison showed that an increasing pressure resulted in a higher derivation between sensor signal (calculated frost point temperature) and reference frost point temperature. At an absolute pressure of 2 bar the differences were minor in consideration of the uncertainty, however at 15 bar the differences were 6.77 K. Nevertheless, it was possible to measure the gas humidity at higher pressure with coulometric trace humidity sensors.
Because ammonia and its reaction products can cause considerable damage to human health and ecosystems, there is a need for reliably operating and reversibly interacting sensor materials to monitor traces of gaseous ammonia in ambient air, which at best can be used on-site for in-the-field measurements. Herein, the development of a sensor material for gaseous ammonia in the lower ppm to ppb range using optical fluorescence as transduction mechanism is presented. A fluorescent dye, which shows reversible fluorescence enhancement in the presence of ammonia is incorporated into a polymer matrix, the latter to ensure the accumulation of ammonia. The sensor material is integrated into a prototype of a miniaturized sensor device, facilitating long-term operation. To calibrate the optical sensor system a gas standard generator, producing standard gas mixtures, is used, leading to a sensitivity down to lower ppm concentrations of ammonia.
Planar coulometric sensors were tested in humidified synthetic air at various gas temperatures. Generated frost point temperature in the gas ranged from -30 °C to -60 °C and were measured by coulometric sensors and in addition by a calibrated dew point hygrometer. The gas temperatures, which were measured by a calibrated Pt100 sensor, were set to -20 °C, 0 °C, 23 °C, 40 °C, 50 °C, and 60 °C during the experiments. Empiric nonlinear functions were calculated between the generated humidity and the sensor signals. In comparison to the measured signals at 23 °C, the sensor signals were lower at the other gas temperatures. The measurements at 60 °C showed indistinct results due to a great signal noise. The response behavior of the sensors was similar at 23 °C, 40 °C and 50 °C. In contrast to that, the sensors reacted slowly at a gas temperature of -20 °C and 0 °C. In summary, with coulometric sensors it was possible to measure continuously trace humidity with an expanded uncertainty below 2 K.
Die Messung der Gasfeuchte im Spurenbereich in unterschiedlichen technisch und medizinisch relevanten Gasen erfolgte mit Sensoren, die auf dem coulometrischen Messprinzip basieren. Die verwendeten planaren coulometrischen Sensoren wurden im Frostpunkttemperaturbereich von -70 °C bis -30 °C in synthetischer Luft, Wasserstoff, Stickstoff und Distickstoffmonoxid (Lachgas) untersucht. Als Referenz für die Messungen wurde ein Präzisionstaupunktspiegel-Hygrometer verwendet. Die Gasfeuchte kann mit Hilfe der Sensoren in allen untersuchten Gasen, aber mit geänderten Kalibrierfunktionen, mit einer erweiterten Unsicherheit von kleiner als 2,1 K bestimmt werden. Für die Messungen in unterschiedlichen Gasen muss also der Einfluss der Gasmatrix auf das Sensorsignal berücksichtigt werden. So ist zum Beispiel bei Messungen in befeuchtetem Wasserstoff, aufgrund von Rekombinationseffekten, ein signifikant geändertes Sensorsignal zu beobachten.
The efficiency of gas sensor application for facilitating the safe use of hydrogen depends considerably on the sensor response to a change in hydrogen concentration. Therefore, the response time has been measured for five different-type commercially available hydrogen sensors. Experiments showed that all these sensors surpass the ISO 26142 standard; for the response times t90 values of 2 s to 16 s were estimated. Results can be fitted with an exponential or sigmoidal function. It can be demonstrated that the results on transient behaviour depend on both the operating parameters of sensors and Investigation methods, as well as on the experimental conditions: gas change rate and concentration jump.