Photoplastic NEMS with an Encapsulated Polysilicon Piezoresistor Nitin S. Kale, Sudip Nag, R. Pinto, V. Ramgopal Rao Centre for Nanoelectronics, IIT Bombay, Mumbai, India Department of Electrical Engineering, IIT Bombay, Mumbai, India. Abstract- We demonstrate a photoplastic NEMS device that has an encapsulated polysilicon piezoresistor. The crucial temperature limitation of depositing a polysilicon film on a polymer was overcome by employing a novel Hotwire CVD process. In this paper, we report the fabrication and characterization of a novel polymeric cantilever with an embedded piezoresistor, which exploits the low Youngs modulus of a polymer and high gauge factor of polysilicon. Such devices are widely used for sensing biochemicals. I. Gas Manifold MFC Exhaust line Filament Assembly LLTC Shaft INTRODUCTION Microcantilever based biosensors have attracted considerable interest to monitor a specific substance in applications such as clinical analysis, environmental control and industrial processes [1]. Adsorption of molecules onto the surface of the cantilever generates a small magnitude (5mN/m to 0.5 N/m) surface stress, resulting in a bending of the cantilever to the tune of a few tens of nanometers [2 - 4]. The detection mechanisms could be optical (measurement of the deflection), or measurement of a change in resonant frequency of the cantilever due to mass change [5], or even piezoresistive (change in resistance due to bending) [6, 7]. Optical readout scheme to measure the deflection of affinity cantilevers suffers from two major problems: (i) realignment of the laser system when performing measurement in liquids that have different refractive index; (ii) measurement is not possible in opaque liquids [3]. On the other hand, in a piezoresistive detection scheme, laser alignment is not required and issues of changing refractive index and processing in opaque liquids simply disappear. As the signal from the piezoresistive detection scheme is an electrical signal, one can build appropriate electronics around it to amplify and process the signal. However, the piezoresistive scheme is less sensitive and noisier than the optical detection scheme [3]. In this paper, for the first time, we present the fabrication and characterization of a novel polymeric cantilever, with an embedded polysilicon piezoresistor. These cantilevers can be used for sensing of biochemicals. The polymer used to fabricate the structural layer and the encapsulation layer was SU-8, which is a negative tone chemically amplified near UV photoresist. It is highly resistant to chemicals and hence can be used as a component material [8]. Also, a method for modification of SU-8 surface has already been invented so as to make it amenable for biomolecule immobilization [9]. Fabricating a structural layer using this material has several advantages: (i) it is a low cost, low thermal budget process in which only spin coating, baking, Reactor Slit Valve Gate Valve View Port Pirani Gauge Fig. 1. HWCVD cluster tool [10] patterning and development is required. Thus one does not need to fabricate a structural layer through a CVD process; (ii) SU-8 has a low Young’s modulus (5 GPa) and thus has a higher propensity for bending, compared to, for example a nitride (150 to 350 GPa), for a given surface stress. II. PHOTOPLASTIC PIEZORESISTIVE DEVICE FABRICATION A. HWCVD Method The critical unresolved technology issue for the integration of a high gauge factor polysilicon material in a SU-8 matrix was the thermal budget limitation of polymers. Both the Lowpressure & Plasma-enhanced CVD processes, normally used for polysilicon deposition, had to be ruled out for polymeric cantilevers because of the temperature limitations. We resolved this crucial issue by employing polysilicon, deposited by the low temperature Hotwire CVD (HWCVD) method, as the piezoresistive material. The figure of the cluster tool for depositing polysilicon (and other films) at a low substrate temperature via the HWCVD process is shown in Fig. 1. The tool can also be employed to modify the surface of SU-8 by attaching amino groups to it via the dissociated ammonia treatment process; and make SU-8 amenable for antibody immobilization. B. Device Fabrication To fabricate the structure, a series of deposit, pattern and etch steps are employed. Fig. 2 (a to m) illustrate the main steps of the 5 mask fabrication process. First, a 2 inch diameter <100> oriented, silicon wafer was cleaned with piranha (1:3 H2O2: H2SO4), followed by the RCA cleaning procedure. 978-1-4244-2104-6/08/$25.00 ©2008 IEEE. Authorized licensed use limited to: INDIAN INSTITUTE OF TECHNOLOGY BOMBAY. Downloaded on January 19, 2009 at 01:39 from IEEE Xplore. Restrictions apply. 460 Silicon dioxide, which was later employed as a sacrificial layer, was then sputtered on the wafer. Next, a 1.8 µm SU-8 2002 layer was spun and patterned on the substrate. This step yielded the bottom layer, i.e. structural layer of the cantilever (Fig. 2(b &i)). Polysilicon was deposited on the SU-8/substrate using the HWCVD process; the substrate heater temperature was maintained at 170 °C [10]. Patterns on the polysilicon film were then defined and the film was etched by dissolving the unprotected polysilicon in HNA (hydrofluoric acid + nitric acid + deionized water). The resultant pattern yielded the piezoresistive polysilicon layer shown in Fig. 2(d & j). thereby further lowering the manufacturing cost. Images of the SU-8/polysilicon/SU-8 piezoresistive cantilevers captured using an optical microscope are shown in Fig. 3. Fig. 3. Optical images of a die with SU-8/polysilicon/SU-8 cantilever (a) single cantilever (b) cantilevers in half-bridge configuration (c) gold pads and track lines (d) entire die III. PHOTOPLASTIC PIEZORESISTIVE DEVICE CHARACTERIZATION Fig. 2. Process sequence to fabricate SU-8/poly/SU-8 cantilevers Next, a 100 nm film of chrome-gold was deposited on the polysilicon/SU-8/substrate. Thus, the appropriately patterned chrome-gold layer formed a contact pad to make an electrical contact with the polysilicon layer (Fig. 2(e & k)). Another layer of SU-8 (thickness was 0.9 µm) that encapsulated the polysilicon was then defined which formed the top layer of the cantilever. Encapsulation of the polysilicon piezoresistor is essential so that the wet biological processes do not short the piezoresistors. The top SU-8 layer is also the immobilization layer of the device. This SU-8 layer can be subjected to hotwire CVD induced dissociated ammonia treatment [9] so as to make it amenable for antibody immobilization. The base of the cantilever die was fabricated using SU-8 2100 which is a highly viscous and therefore ‘thick’ negative photoresist (Fig. 2(g & m)). The die was released from the substrate by etching the sacrificial (sputtered) oxide in hydrofluoric acid (Fig. 2(h)). When the acid dissolved the oxide completely, the dies simply lifted off from the substrate. An important advantage of this method is that it does not ‘consume’ the substrate as in surface or bulk micromachining. Hence the substrate is reusable, Mechanical characterization of the cantilever was performed to measure its stiffness. Electromechanical characterization of the cantilever was performed to quantify the change in resistance of one of the levers for a given deflection at its tip. Stiffness characterization of the cantilever was performed by the technique developed by Serre et al [11]. The technique is based on the measurement of the deflection of the tip of the sample cantilever; due to a load applied on it, by an AFM cantilever. Molecular Imaging AFM was used to measure the stiffness (i.e. its spring constant) of the SU8/polysilicon/SU-8 cantilever. The AFM cantilever chosen was a silicon nitride structure whose nominal stiffness was 0.12 N/m (i.e KAFM=0.12 N/m). The AFM cantilever was made to approach the tip of the SU-8/polysilicon/SU-8 cantilever. To obtain the approach curve i.e. the ‘AFM Force vs Distance spectroscopy’ the deflection vs distance sweep was run. The plot for the approach curve i.e. ‘Force vs distance spectroscopy’ as the AFM cantilever approaches the SU8/poly/SU-8 cantilever is shown in Fig. 4(a). This information used in conjunction with the ‘calibrate’ software tool of the AFM is used to extract the deflection of the AFM tip in nanometers per Volt. The calibration information is also depicted in the text box as y = - 0.026 + 5.85. Next, the measurement involving actual bending of the probe cantilever i.e. ‘AFM Calibrated Force vs Distance Spectroscopy’ was carried out. The deflection of the AFM cantilever in nanometers (nm) plotted as a function of the distance traveled by the scanner tube (in nm) is shown in Fig. 4(b). Using the stiffness data of the AFM cantilever (KAFM=0.12 N/m) we 461 Authorized licensed use limited to: INDIAN INSTITUTE OF TECHNOLOGY BOMBAY. Downloaded on January 19, 2009 at 01:39 from IEEE Xplore. Restrictions apply. calculate the spring constant or stiffness of the SU-8/poly/SU-8 cantilever to be 0.25 N/m. nulled node. This clearly established a piezoresistive behaviour by the encapsulated polysilicon layer. y = -0.026x + 5.85 Fig. 4(a). AFM Force vs distance spectroscopy Fig. 5. Change in voltage across the deflected cantilever vs deflection at the tip of the cantilever. Therefore, we have successfully characterized the fabricated polymer cantilever that has an encapsulated polysilicon piezoresistor. Its stiffness was determined. For its electromechanical characterization, one of the two cantilevers of the die, that formed a balanced (and nulled) half bridge, was deflected and a change in voltage across it was measured, thereby establishing piezoresistive behaviour. y = 0.673x + 292.87 Fig. 4(b). AFM Calibrated Force vs Distance Spectroscopy An important performance parameter of a piezoresistive cantilever is its deflection sensitivity. It is a measure of the relative change in resistance as a function of cantilever deflection. The measurement is performed by deflecting the sample cantilever by a micromanipulator. The relative change in resistance is measured using a highly sensitive in house developed electromechanical characterization system. Three micromanipulators of a Karl Suss PM8 probe station were used to probe the three gold pads, while the 4th micromanipulator of the probe station was used to deflect the cantilever. The plot of the measured change in voltage as the cantilever is deflected is shown in Fig. 5. We observed that the voltage measured at the measurement node changed as the cantilever was deflected. This occurred because the deflected cantilever got strained; due to which its resistance changed, thus causing a ‘voltage measure’ at the previously Thus we demonstrate, for the first time, a photoplastic NEMS device that has an encapsulated polysilicon piezoresistor. The device is designed and fabricated so that it can fit into the nose of an AFM; therefore it can be used in conjunction with an AFM’s liquid cell for biochemical sensing applications. Antibodies, such as anti-myoglobin, can be immobilized on one surface of the cantilever inside the AFM’s liquid cell. The scheme can be used to detect myoglobin, a cardiac marker, which is released when a person has a heart attack. 5. CONCLUSION In this paper we have reported, for the first time, the fabrication of a polymeric microcantilever with an encapsulated polysilicon piezoresistor, using a 5 mask process. The process to fabricate the die was developed in such a way that it can be lifted off the silicon substrate. Hence the silicon substrate is reusable. The polysilicon piezoresistor is fully encapsulated by SU-8, so that the wet biological processes do not short the piezoresistors. The devices were characterized for their mechanical and electro-mechanical behaviour. The spring constant of the fabricated SU-8/polysilicon/SU-8 cantilevers was measured to be 0.25 N/m. The piezoresistive properties of these cantilevers with an encapsulated HWCVD polysilicon piezoresistor, were demonstrated and characterized. 462 Authorized licensed use limited to: INDIAN INSTITUTE OF TECHNOLOGY BOMBAY. Downloaded on January 19, 2009 at 01:39 from IEEE Xplore. Restrictions apply. ACKNOWLEDGMENT Nitin S. Kale gratefully acknowledges the financial support provided by the National Program on Smart Materials and Structures and the Nanotechnology project; both funded by the Government of India. REFERENCES [1] R. Raiteri , M. Grattarola M, H. Butt, P. Skaldal, “Micromechanical cantilever based biosensors”, Sensors and Actuators B 79 (2001) p. 115. [2] J. Fritz et al, “Translating biomolecular recognition into nanomechanics”, Science 288 (2000), p. 316. [3] J. Thaysen, “Cantilever for biochemical sensing integrated in a microliquid handling system”, Ph D Thesis, Technical University of Denmark (2001). [4] Y. Arntz et al, “Label free protein assay based on a nano mechanical cantilever array”, Nanotechnology 14, pp 86 (2003). [5] F. Battiston et al, “A chemical sensor based on a microfabricated cantilever array with simultaneous resonance frequency and bending readout”, Sensors and Actuaors B 77 (2001) p. 122. [6] R. Berger et al, “Micromechanical thermogravimetry”, Chemical Physics Letters 294(4&5) (1998), p. 363. [7] H. Jensinius e al, “A microcantilever based alcohol vapor sensor application and response model”, Appl. Phys. Lett. 76(18) (2000), p. 2615. [8] J. Shaw, J. Gelorme, N. LaBianca, W. Conley, S. Holmes, “Negative photoresists for optical lithography”, IBM Journal of Res & Dev (Optical Lithography) (1997) 41(1/2). [9] IIT Bombay, “A novel dry method of surface modification of SU8 for immobilisation of biomolecules using hotwire induced pyrolytic process. Indian Patent No. 213504 Indian Patent Office (2004). [10] N. Kale, “Making Hotwire CVD a Viable Technology Alternative for BioMEMS Applications: Device Optimization, Fabrication and Characterization” Ph D Thesis, IIT Bombay (2008). [11] C. Serre et al, “Measurement of micromechanical properties of polysilicon microstructures with an atomic force microscope”, Sens and Act A 67 (1998), p. 215. 463 Authorized licensed use limited to: INDIAN INSTITUTE OF TECHNOLOGY BOMBAY. Downloaded on January 19, 2009 at 01:39 from IEEE Xplore. Restrictions apply.
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