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A Chemocapacitive sensor array for the detection of complex odors. D. Goustouridis 1,2 , P. Oikonomou 2 , A. Botsialas 1,2 , K. Manoli 2 , M. Kitsara 2 , I. Raptis 2. Overview. Polymer based gas sensors Principles of operation Capacitive Polymer Based sensors
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A Chemocapacitive sensor array for the detection of complex odors D. Goustouridis1,2, P. Oikonomou2, A. Botsialas1,2, K. Manoli2, M. Kitsara2, I. Raptis2
Overview • Polymer based gas sensors Principles of operation • Capacitive Polymer Based sensors Methodology for the selection of the Polymers Fabrication of the sensor array • Capacitance measurement set-up Capacitance measurements • Read-out electronics Capacitance measurements • Applied Algorithms Applications • Conclusions – Future Plans 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Chemical sensors • Piezoelectic (surface acoustic waves SAW, bulk acoustic waves BAW, cantilever resonator) • Optical (fluorescence, reflective, absorption) • Thermal (pellistor) • Electrical, Electrochemical ( chemoresistive, MOX, chemocapacitive) 2nd SENS-ERA Workshop, 5-6 Dec. 2012
InterDigitateElectrode (IDE) Capacitive Sensor h Sensitive Layer + - + Electrode Substrate G W λ Top view Side view • Simple and low cost fabrication • Suitable for parallel production • Low power consumption • Promising devices for sensing VOCs or humidity • Could be integrated with read-out electronics 2nd SENS-ERA Workshop, 5-6 Dec. 2012
IDE Chemocapacitor sensing principle Vapor phase h Sorbed molecules + - + Polymer sensitive layer Electrode Substrate λ Change in permittivity of polymer (ΔCε ): i) ΔCε >0, εA(analyte)>εpol(polymer) ii) ΔCε <0, εA(analyte)<εpol(polymer) Capacitance change (ΔC) Sorption of analyte ΔC= f( ΔCε + ΔCh) Swelling of polymer (ΔCh): ΔCh>0 ΔCh~0 if i) h>0.5 λ,ii)εΑ>> εpol for any h 2nd SENS-ERA Workshop, 5-6 Dec. 2012
IDE Chemocapacitor sensing principle Useful Capacitance Electric Field ΔCh: Capacitance change due to swelling ΔCε: Capacitance change due to permittivity change Parasitic Capacitance • Requirements: • Substrate with low dielectric constant (Polymer or Quartz) • Small electrode distance (ideally <1μm) 2nd SENS-ERA Workshop, 5-6 Dec. 2012
IDE Chemocapacitor operating principle Α) Response of chamocapacitor in neutral enviroment, Β) Just before the first sorption Γ) After the sorption, transiet response Δ)Steady response in equilibrium 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Development of an e-nose • Choosing of the polymers for gas sorption • Choosing of group of polymer (according to specific application) (Compatibility with the measuring gases, chemical affinity, technological issues, …) • Control of sorption – desorption, repeatability, selectivity • Transducer & Sensor Development • Deposition techniques • Implementation of Interdigitated Electrodes & characterization. • Read-Out electronics • Development of read-out electronics and data transmittion modules • Development of Data processing algorithms • Application of raw data processing algorithms for the identification of the gas composition. 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Optical Characterization of the polymer swelling Measurement chamber Symbolemtry principle of operation • The energy E at wavelength λ is (for the case of single layer film): • n : Refractive index, L: thickness, λ: wavelength.με 0: πολυμερές 1:. • 0 indicates the polymer layer & 1 the SiO2 layer • Fitting (L0) of theoretical spectrum to the measurement one. White Light Reflectance Spectroscopy (WLRS) 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Optical Characterization of the polymer swelling Analyte atmosphere (swelling more) Analyte Atmosphere (swelling) Nitrogen purging Polymer SiO2 Si 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Typical Results Thickness (nm) Time (min) Polymer film: PHEMA Analyte: Humidity Concentrations: 1000-5000-10000-15000-20000 ppm 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Fabrication process of IDC Array Plan view of IDC structure Array of 8 chemopapacitors 2μm electrode – 2μm spacing (die size 7x7mm2) 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Measurement Set-up • Gas delivering unit • Sample’s chamber (volume ~4mm3) • Eight channel matrix switch board (Capacitance meter (HP 4278A) • The set-up is completely controlled by a LabView application Capacitance change (pF) Time(min) 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Measurement set-up 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Response to concentrations of two analytes • Δcdouble.~(ΔCanalyte1+ ΔCanalyte2) • The sensors sense the present or the absent of each analyte. 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Aging through time 4 months later • Good reproducibility and reversibility • Time stability 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Read out & Electronic Module Electronic circuit for up to 8 Chemocapacitance reading 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Typical results of Electronic Module Mesurement of p-xylene(100ppm) with & without Humidity 2nd SENS-ERA Workshop, 5-6 Dec. 2012
PCA analysis Processing of the raw data 2 or 3 axes representation (the most important) Principal Component Analysis (PCA) 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Application I. Wine discrimination 3- Agiorgitiko- red - boutari 4- Naousa-red - boutari Discrimination of white & red wine 1- Limnoswhite dry 2-Moschofilero-white Απόκριση του αισθητήρα PBMA-IDC στα τέσσερα κρασιά για δυο ροές Αποτέλεσμα PCA 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Application II: Fragmentation monitoring Response of 2 IDC vs time Fragmentation vs time according to PCA analysis 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Conclusions • Methodology • Development of Methodology for the characterization of polymer based chemocapacitors • Polymeric Films • Characterization of polymers films for odors sensing • Chemocapacitors Array • Development of implementation techniques of chemocapacitos • Implementation & characterization of chemocapacitos Array • Read out electronics • Development of a hybrid system of chemocapacitors array with appropriate read-out electronics • Λογισμικό ανίχνευσης αερίων • Λογισμικό PCA • Εφαρμογές • Ζύμωση γλεύκους 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Future plans Δίκτυο • Development of submicron IDCs. • Apply pattern recognition algorithms • Implementation of a wireless network • Measurements in real environment. 2nd SENS-ERA Workshop, 5-6 Dec. 2012
Thank you for your attention E-mail: dgousto@teipir.gr 2nd SENS-ERA Workshop, 5-6 Dec. 2012