DOI 10.5162/IMCS2012/P2.2.12 Design and Implementation of a High-Frequency Surface Acoustic Wave Sensor Array for Pheromone Detection in an Insect-inspired Infochemical Communication System S. Thomas, S. Li Tai Leong, Z. Rácz, M. Cole, and J.W. Gardner Microsensors & Bioelectronics Laboratory, University of Warwick, Coventry, United Kingdom, J.W.Gardner@warwick.ac.uk Abstract This paper reports on the design and development of a novel pheromone detection biosensor module that forms part of an infochemical communication system. Infochemical communication in insects is based upon the use of sex pheromones for the tenacity of attracting conspecific mates. Our system involves three functional blocks: a chemoemitter module comprising a high-precision syringe pump and a micro-machined artificial gland; a chemoreceiver module comprising an array of four polymercoated dual Surface Acoustic Wave Resonator (SAWR) sensors with associated oscillator drive circuitry; located inside a small odour chamber. Chemical information takes the form of insect pheromone compounds that are released inside the odour chamber by a silicon-based microevaporator and then detected by the sensor array. The design and fabrication of a high frequency 262 MHz oscillator circuit is described giving stable Surface Acoustic Wave (SAW) signals with reference SAWRs used to offset drift. Key words: SAWR Sensors, pheromone, infochemical communication, high frequency, oscillator circuit. Introduction It is of fundamental significance for a wide variety of living organisms to exchange molecular information and process it in a unique way. Intraspecific communication in insects is achieved by the use of semiochemicals; these odour cues are able to modify behavior such as conspecific mate finding, location of food, and other social interactions [1]. This is due to the fact that, for example, moths utilize their olfactory system that enables them to translate odour signals to a complex behavioural pattern within the antenna lobe, which is at the bottom of the detecting organ (antenna). The work presented here mimics chemical communication in insects in which a female moth releases a sex pheromone and the male moth detects it remotely and arises from an EUfunded Framework project called “iCHEM” [2]. Pheromones play an important role in the behaviour of an insect by triggering a preencoded behaviour that enables the male to locate the calling female. These pheromone components, usually released by the female moths as a blend of different compounds, are biosynthesized in the insect‘s pheromone gland. Fig. 1. Schematic block diagram of the biosynthetic insect-inspired communication system. In order to accomplish species-specificity, these pheromone components are blended with variation in molecular chain length, unsaturation level, functional group and total number of compounds. The olfaction system of the moth Spodoptera littoralis has been studied extensively in recent years, both from a behavioral and neurophysiological view [3]. Since (Z,E)-9,11-tetradecadienyl acetate (ZE9,11- 14:OAc) forms the main component in the sex pheromone of this moth [4], we have employed this pheromone compound for the establishment of insect-based communication protocol in our work. IMCS 2012 – The 14th International Meeting on Chemical Sensors 1440 DOI 10.5162/IMCS2012/P2.2.12 Figure 1 shows a schematic block diagram that is analogous to pheromone communication of insects. Our experimental set-up consists of a chemoemitter that generates a set of semiochemical signals, an odour chamber simulating a wind tunnel and a piezoelectric chemoreceiver containing an array of SAWR sensors coated with different types of polymers. The differential signal generated by the SAWR sensors produce varied responses allowing us to detect and decode the pheromone mixtures. Insect-inspired Communication System I. Biosynthetic Pheromone Emission The artificial pheromone-emitter gland is driven by a syringe pump and an evaporation controller system used to control a micromachined evaporator [5] for the release of pheromone into the chamber. This artificial gland imitates the functionality of the biological mechanism that allows the moth S. littoralis to release pheromones in specific dosing. Our chemoemitter is crucial for the labeling of information before they are transmitted into the real world based on relative proportions between compounds [5]. As the normal solution of pheromone Z,E-9,1114:OAc is highly concentrated, hexane was used as the solvent for diluting the pheromone. The microevaporator temperature was set to a temperature of 90°C and different volumes of this pheromone solution was delivered to the chip by a syringe pump at a flow rate of 5 µL/sec, in order to input the odour stimulus into the wind tunnel. II. Fig. 2. Photograph of a dual 262 MHz SAW resonator sensor with surface mount amplifier, filter and buffer circuitry. The X-propagating ST-cut quartz based gas phase dual SAW Resonator sensors with aluminum electrodes are designed to resonate at 262 MHz in a feedback loop of a simple radio frequency (RF) oscillator circuit. The design specifications of the SAWR are 60.5 pairs of interdigitated transducers (IDTs) with 3 µm finger width, acoustic aperture of 720 µm and a cavity length of 1764 µm. 550 reflector gratings surround the IDTs for creating a standing wave pattern. Figure 2 shows the photograph of the dual 262 MHz SAWR sensor with surface mount oscillator circuitry. Chemoreception using SAWR Sensors A highly-sensitive (ppb level), polymer-coated RF-based SAWR oscillator array was employed to detect the semiochemical concentrations in the gas phase, which electronically simulates the complex olfactory system of the night-active insects. More specifically, the SAWR sensor array mimics the insect’s antenna with different types of sensilla designed for detection of various olfactory stimuli [4]. The SAW resonator based sensors are not only highly sensitive, but also simpler in operation having only frequency output and so require a much simpler interface circuitry for data processing. The dual SAWR arrangement enables the generation of differential signals that help ameliorate common mode variations, e.g. drift. Fig. 3. Schematic diagram of the SAWR sensor coated with a polymer based functional layer and exposed to gas molecules. Four different polymers, namely polycaprolactone (PCL), poly(9-vinylcarbazole) (PVK), poly(styrene-co-butadiene) (PSB) and poly(ethylene-co-vinyl acetate) (PEVA) were recognized as the optimal polymers that were stable, reasonably sensitive and selective to the insect pheromones. Therefore, one side of each dual SAWR was functionalized with these polymers (schematic shown in figure 3) while the other side served as a reference, thus enabling the decryption of the encoded information. Figure 4 [A] shows an optical microscopy image specifying the locus of the polymer coating on a dual SAWR sensor and figure 4 [B] shows the magnified view of the polymer coating. IMCS 2012 – The 14th International Meeting on Chemical Sensors 1441 DOI 10.5162/IMCS2012/P2.2.12 Fig. 4 [A]. Optical micrograph specifying the locus of the polymer coating on one side of a dual SAWR sensor [B]. Magnified view of the polymer coating. III. resonator. Therefore the circuit employs a commercial high gain monolithic microwave integrated circuit (MMIC) wide-band amplifier µPC2710 (NEC), having a gain of 33 dB, with a maximum input power of 10 dBm and a maximum output power of 13.5 dBm allowing the device to be operated safely with a loop loss of 3.5 dB or more. The low pass filter consisting of passive elements suppresses the oscillations at other spurious frequencies. A commercial bipolar MMIC wide band amplifier µPC2711 (NEC) forms the buffer stage with a gain of 13 dB in order to measure the differential analogue oscillator output signal. Oscillator Circuit Design The SAWR sensors were driven by amplifier based independent feedback-oscillator circuits consisting of surface mount amplifiers, a low pass filter, and the buffer circuitry. The oscillator Printed Circuit Board (PCB) is a four layer board with separate grounding planes which takes account of the phase shifts associated with the RF signal path within the resonatorcircuitry loop. It also reduces the RF cross talk, thereby improving noise sensitivity. A schematic layout of the RF oscillator circuit is shown in Figure 5 comprising low pass filter, amplifier and buffer stages. Fig. 6. Attenuation vs. frequency plot for a 262 MHz SAW resonator Sensor. Experimental Setup Fig. 5. Schematic diagram of circuitry to drive the SAWR sensor and buffer the read-out signal. The SAWR devices are used as the frequency and phase selective elements in the feedback loop of the oscillator circuit because they provide a maximum signal transmission at the designed frequency (262 MHz) with very low, typically 12 dB attenuation as indicated by the scattering parameter analysis in figure 6. In addition to the SAWR attenuation, approximately 2 dB is also lost through the filters and cables in the circuit. The amplifier gain should always exceed the total signal loss in the feedback loop of the oscillator circuit elements by a typical gain margin of 5 dB [2], for maintaining a stable operation of the SAWR Fig. 7. Test chamber containing pheromone microevaporator and array of four polymer-coated SAWR sensors. A prototype of the insect-based pheromone detection system has been constructed as shown in the figure 7. The chemoemitter module consists of a neMESYS high-precision dual channel syringe pump (cetoni GmbH, Germany) that drives a micro-machined artificial gland, releasing pheromone into the 14x14x40 3 cm Perspex odour chamber. The polymer coated 4-sensor dual SAWR array, with the related RF oscillator circuitries and interfaces make up the chemoreceiver module. Using a IMCS 2012 – The 14th International Meeting on Chemical Sensors 1442 DOI 10.5162/IMCS2012/P2.2.12 commercial FQ4 interface instrument (JLM Innovation, Tubingen, Germany) and a desktop computer within the experimental system, the output of each sensor was measured and recorded independently. Results In this paper we have shown the response of a SAWR sensor array to a biosynthetic pheromone compound and the development of a custom high-frequency oscillator circuit to drive four dual SAWR sensors. The differential frequency response of the polymer coated SAWR sensors to the pheromone was successfully measured as shown in Figure 8. Fig. 8. Differential frequency response of four different polymer-coated SAWR sensors to pheromone Z,E-9,11-14:OAc. In random repeated sequences, 5, 10, 15 and 20 µl of a solution of Z,E-9,11-14:OAc (10% volume in hexane) were introduced into the odour chamber using the microevaporator and the responses obtained were approximately linear (see Figure 9) and can be classified using a simple linear statistical classifier. Moreover, it can be also observed that variations in blend concentrations are clearly visible and separable as well. This also proves that the pheromones can be transmitted and detected by the different SAWR sensors. Thus proportionately-encoded signals can be transmitted in our infochemical communication system. Conclusions We have presented an integrated chemoemitter and chemoreceiver system that simulates infochemical communication in insects, thereby forming a new branch of expertise for information transmission using only molecules. The differential sensor outputs can be directly fed into a field-programmable gate array for neuromorphic signal processing permitting autonomous robot control for search and rescue, and has become an intricate scheme for encoded message transmission. In addition to providing the required selectivity that is necessary for pheromone blend specificity, the SAW sensors offer low-cost and low-power, and offer a route to full CMOS integration with the driving, data acquisition and processing circuitry. Future development of this work is being directed towards testing and optimizing the capability of the system to generate and detect a precise mix of pheromone compounds in programmable ratios of concentration. Moreover, further advances include the integration of the olfactory sensor drive and interface circuitry into an application-specific integrated circuit (ASIC) chip boosting them to full system-on-chip (SoC) implementation of chemoreceiver system. Acknowledgements This work was supported by the EC 6th Framework Programme, and FET project no. FP6-032275 called “Biosynthetic Infochemical Communication”. References [1] E. Hartlieb, et al., “Appetitive Learning of Odours With Different Behavioural Meaning in Moths,” Physiology & behavior, vol. 67, no. 5, 671-677 (1999). [2] iCHEM Project, EU FP6 STREP project, see www.go.warwick.ac.uk/iCHEM [3] R. J. Fan and B. S. Hansson, “Olfactory Discrimination Conditioning in the Moth Spodoptera littoralis,” Physiology & behavior, vol. 72, no. 1-2, 159-165 (2001). [4] P. Anderson et al., “Increased Behavioral and Neuronal Sensitivity to sex Pheromone After Brief Odor Experience in a Moth,” Chemical senses, vol. 32, no. 5, 483-491 (2007); doi:10.1093/ chemse/bjm017 [5] W. P. Bula et al., “Artificial Gland for Precise Release of Semiochemicals for Chemical Communication,” 14th International Conference on Miniaturized Systems for Chemistry and Life Sciences, 671-673 (2010). Fig. 9. Response of four polymer coated SAWR sensors to different volumes of odour pulse. IMCS 2012 – The 14th International Meeting on Chemical Sensors 1443