Poster Session, Thursday, June 17Theme F686 - N1123Humidity Sensor applications based on Carbon Nanotubes (CNTs) modified with various Calixarenemolecules measured by a Quartz Crystal Microbalance (QCM)F. Nadi Gür 1* , S. Okur 1* , Nesli T. Yağmurcukardeş 1 , Mustafa Yılmaz 2 , Mahmut Kuş 31 Izmir Institute of Technology, Department of Physics Urla/Izmir/TURKEY2 Selçuk University, Department of Chemistry, Selçuklu/Konya/TURKEY3 Selçuk University, Department of Chemical Eng<strong>in</strong>eer<strong>in</strong>g, Selçuklu/Konya/TURKEYAbstract— We predict that CNTs modified with calixerene molecules has a strong potential to <strong>in</strong>vestigate as a humiditysensors. This study focuses on humidity sens<strong>in</strong>g properties of CNTs modified with calixrene. The humidity adsorbtiondesorptionk<strong>in</strong>etics are tested by Quartz Crystal Microbalance (QCM) technique. Accord<strong>in</strong>g to the our experimental results,modified CNTs with calixerene film will be possible option and open new approaches for more reliable, high sensitive,reversible and cost effective electro-chemical sensor applications.The accurate measurements of humidity levels are veryimportant concerns <strong>in</strong> environmental fields, such as medical ordomestic applications for human comfort, <strong>in</strong>dustrial uses,agriculture, automobiles.Thus, the requirement for cheap,reliable and sensitive sensors are urgent.Across all over the world, researchers have been<strong>in</strong>terested <strong>in</strong> CNT based sensors and CNTs have shown to bestrong potential for the revolutionary of sensors generations[1]. As can be seen from Fig.1, due to their small size, highstrength, high electrical and thermal conductivity, and largeeffective active area, CNTs have many advantages compare tothe bulk or th<strong>in</strong> films for electro-chemical sensor applications[1,2].repeatability characteristics. The adsorption-desorptionk<strong>in</strong>etics are analyzed and discussed <strong>in</strong> details. F (Hz)50%110 %22 (a)%43-50 %53-100-150%75%84%94 %94%75%84%11%22%43%53-200%97-2500 1000 2000 3000 4000 5000 6000Time (s)- F (Hz)1000100 F (Hz)500-50-100-150-200(b)%43%53%75%84%97-2500 200 400 600 800 1000 1200Time (s)y = 13.733 * e^(0.028238x) R= 0.99383y = 8.1544 * e^(0.034337x) R= 0.98145(c)downwardupwardFigure 1: SEM image of carbon nanotubes filmTh<strong>in</strong> films of calixarene derivatives have been widely used<strong>in</strong> chemical sensors. Due to their zeolite-like capacity andselectivity, calixarenes became promis<strong>in</strong>g materials for sensorapplications [3]. Calixarene derivatives have been used <strong>in</strong>recent times as gas sensors applications [4]. It is also knownthat some calixarene derivatives adsorb water molecules. SalihOkur reported a humidity sens<strong>in</strong>g properties of calixerenederivatives [5]. However we did not reach any application ofCNTs modified with calixerene molecules based on humiditysensor.QCM tehnique is a powerfull option to <strong>in</strong>vestigate sens<strong>in</strong>gproperties of modified CNTs, s<strong>in</strong>ce it is highly sensitive tomass changes 1 ng/ 2 [2]. QCM has been used widely tomonitor the change <strong>in</strong> mass load<strong>in</strong>g by measur<strong>in</strong>g the shift ofits resonant frequency [5].In this work, we firstly started with CNTs dissolved <strong>in</strong>toethanol and CNT film coated by drop-cast<strong>in</strong>g technique.Humidity measurements of CNT film were recorded andmonitored by QCM from %11 RH to %97 RH. Accord<strong>in</strong>g toFig.2 adsorbtion-desorbtion process are very fast andreversible. We have obta<strong>in</strong>ed very good response and high1020 30 40 50 60 70 80 90 100Relative Humidity (%)Figure 2: QCM frequency shifts (Hz) as a function of time (s) for different<strong>in</strong>creas<strong>in</strong>g and decreas<strong>in</strong>g relative humidity values between 11% and 97% RH(a) and (b) The change <strong>in</strong> the QCM frequency vs vary<strong>in</strong>g RH values (c)In summary, both CNTs and Calixerene derivates show verygood response to humidity changes sensor applications.Modified CNTs with Calixerene molecules show highlysensitive responce to RH changes and can be used as costeffective sensor materials.*Correspond<strong>in</strong>g author: salihokur@iyte.edu.tr ,fatihnadigur@gmail.com[1] Niraj S<strong>in</strong>ha, Jiazhi Ma, and John T. W. Yeow, Carbon Nanotube-BasedSensors,JNN Vol.6, 573–590, 2006[2] Y. Zhang, K. Yu, R. Xu, D. Jiang, L. Luo, Z. Zhu, Quartz crystalmicrobalance coated with carbon nanotube films used as humidity sensor,Sens. Actuators A 120 (2005) 142–146.)[3] Koshets I. A., et.al.,Sens. Actuators B 106, (2005), 177[4] Ohira, Sh<strong>in</strong>-I. , et.al., Talanta 2009, 77, 1814.[5]Salih Okur, Mahmut Kus, Faruk Ozel, Mustafa Yılmaz,Humidityadsorption k<strong>in</strong>etics of water soluble calix[4]arene derivativesmeasured us<strong>in</strong>g QCM technique,Sensors and Actuators B 145 (2010) 93–976th Nanoscience and Nanotechnology Conference, zmir, 2010 699
Poster Session, Thursday, June 17Theme F686 - N1123Investigation of Humidity Sens<strong>in</strong>g Properties of ZnS NanowiresS.Okur 1 , N.Tekgüze1 1 l, A. Erol 2 , N.Üzar 2 , M.Ç. Arıkan 21 Izmir Institute of Technology, Faculty of Science, Department of PhysicsGülbahce Koyu Kampüsü, Urla, Izmir,35430, Turkey2 Istanbul University, Science Faculty, Physics Department, Vezneciler, 34134 Istanbul, TurkeyAbstract— ZnS nanowires synthesized by the VLS (Vapor-Liquid-Solid) method and were <strong>in</strong>vestigated by Quartz Crystal Microbalance (QCM)method and electrical measurements. The synthesized nanowires were exposed to relative humidity (RH) between 33% and 100% undercontrolled environment. Our experimental results show that ZnS nanowires have a great potential for humidity sens<strong>in</strong>g applications for roomtemperature operations.Semiconductor nanostructures have attracted great attention asmaterials for sens<strong>in</strong>g gases and humidity due to their superior sens<strong>in</strong>gfeatures such as very high surface to volume ratio, lower cost and easeto fabricate as a sensor compared to bulk or th<strong>in</strong> films [1]. Sens<strong>in</strong>g andcontroll<strong>in</strong>g of humidity is very important for many manufactur<strong>in</strong>genvironments such as food, automotive and electronics <strong>in</strong>dustries. ZnSnanostructures should be used as humidity and gas sensor due to theirhighly active surface properties.In this work, we explored the humidity sens<strong>in</strong>g capability of ZnSnanostructures us<strong>in</strong>g QCM method, at which the measured frequencyshift is directly proportional to the mass change on a quartz crystal [2],and electrical measurements such as voltage-current (I-V), resistance-RH% and capacitance-frequency (C-f) from 33% RH to 100% RH.ZnS nanostructures were synthesized us<strong>in</strong>g VLS technique. Fig.1shows the morphology of the synthesized nanostructures is nanowireswith their diameters range from 60 nm to 300nm.decreases almost l<strong>in</strong>early with <strong>in</strong>creas<strong>in</strong>g RH. This decreas<strong>in</strong>g ofresistance was about four orders. Typical I-V curves of ZnS nanowiressensor from 33% RH to 100% RH are shown <strong>in</strong> Fig.3b. These I-Vcurves are a straight l<strong>in</strong>e, show<strong>in</strong>g ohmic behavior. Molecules ofmoisture <strong>in</strong>teraction with semiconductor surfaces <strong>in</strong>fluence surfaceconductivity due to physical and chemical adsorption of watermolecules. Charge exchange occurs between adsorbed species from themoisture and the semiconductor surface. Conductivity of ZnSnanowires sensor <strong>in</strong>creases with <strong>in</strong>creas<strong>in</strong>g relative humidity is relatedto amount of the absorption of moisture molecules on the surface ofZnS nanowires sensor.Resistance (Ohm)10 1110 1010 910 810 7y = 6,9462e+11 * e^(-0,11993x) R= 0,96093B10 12 30 40 50 60 70 80 90 10010 610 5Fig. 1: SEM image of the ZnS nanostructuresIn order to monitor humidity sens<strong>in</strong>g properties, ZnS isultrasonically dispersed <strong>in</strong> ethanol and solution was applied on thesurface of quartz crystal and between the two gold (Au) electrodes bydrop-cast<strong>in</strong>g technique for QCM and electrical measurements,respectively. The dropped solution was dried at room temperature untilethanol was totally evaporated. The quartz crystal and electrodesloaded with ZnS nanowires were exposed to the relative humidity at thesame time. Fig. 2 shows the frequency shift of ZnS loaded QCM crystalunder vary<strong>in</strong>g relative humidity (RH) between 45 and 75% for fourhumidity adsorption/desorption cycles. Dur<strong>in</strong>g the adsorption ofmoisture molecules on the sensor surface the frequency shift decreaseswith <strong>in</strong>creas<strong>in</strong>g RH and goes to near saturation values, while frequencyshift decreases dur<strong>in</strong>g the desorption. This is why ZnS nanowiresposses a large specific surface area, moisture molecules adsorb easilyon the sensor surface and the mass of quartz crystal <strong>in</strong>creases with<strong>in</strong>creas<strong>in</strong>g RH.dF/Hz0-200-400-600-800-1000dF/Hz Relative Humidity (%)400 200 400 600 800 1000 1200 1400Fig. 2: The frequency responses of an loaded QCM with drop-casted ZnSnanowires (red squares) compar<strong>in</strong>g with relative humidity values of acommercial sensor (blue circles) for 4 humidity adsorption-desorption cyclesbetween 45% and 75% RH.Fig.3a shows the resistance variation of ZnS nanowires depend<strong>in</strong>gon vary<strong>in</strong>g relative humidity. The resistance of ZnS nanowiresTime (s)8075706560555045Relative Humidity (%)Current (A)Relative Humidity (%)A0,020,0150,010,0050-0,005-0,01-0,015100 33%-0,02-6 -4 -2 0 2 4 6bVoltage (V)Fig. 3: a) The resistance variation, b) the I-V characterization of ZnS nanowiresunder vary<strong>in</strong>g relative humidityIn summary, the QCM and electrical measurements resultsshow that ZnS nanowires can be used for potential humiditysensor application.*Correspond<strong>in</strong>g author:neslihanuzar@istanbul.edu.tr.[1] D.P: Norton, Y.W. Heo, M.P. Ivill, K. Ip, S. J. Pearton, M. F. Chisholm, T.Ste<strong>in</strong>er, Materials Today, 34, 7, (2004)[2] Lukas Schmidt-Mende and Judith L. MacManus-Driscoll, 10, 40-48, 2008.90% %4384% 55%75%55% 84%90% 43%100% 33%6th Nanoscience and Nanotechnology Conference, zmir, 2010 700
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