Elsevier

Sensors and Actuators B: Chemical

Volume 208, 1 March 2015, Pages 600-607
Sensors and Actuators B: Chemical

Geometry optimization of uncoated silicon microcantilever-based gas density sensors

https://doi.org/10.1016/j.snb.2014.11.067Get rights and content

Abstract

In the absence of coating, the only way to improve the sensitivity of silicon microcantilever-based density sensors is to optimize the device geometry. Based on this idea, several microcantilevers with different shapes (rectangular-, U- and T-shaped microstructures) and dimensions have been fabricated and tested in the presence of hydrogen/nitrogen mixtures (H2/N2) of various concentrations ranging from 0.2% to 2%. In fact, it is demonstrated that wide and short rectangular cantilevers are more sensitive to gas density changes than U- and T-shaped devices of the same overall dimensions, and that the thickness does not affect the sensitivity despite the fact that it affects the resonant frequency. Moreover, because of the phase linearization method used for the natural frequency estimation, detection of a gas mass density change of 2 mg/l has been achieved with all three microstructures. In addition, noise measurements have been used to estimate a limit of detection of 0.11 mg/l for the gas mass density variation (corresponding to a concentration of 100 ppm of H2 in N2), which is much smaller than the current state of the art for uncoated mechanical resonators.

Introduction

In recent years microcantilever-based chemical, biological and physical sensors have attracted the interest of numerous researchers due to their high surface-to-volume ratio and their high performance in both gas and liquid phases [1], [2], [3], [4], [5], [6]. For chemical and biochemical sensing applications, the microcantilevers are usually coated with a sensitive layer whose purpose is to selectively sorb the analyte of interest, resulting in either a static deflection (bilayer effect) in the static mode or a shift in the resonant frequency (mass effect) in the dynamic flexural mode. Furthermore, it has been demonstrated that uncoated micro- or millimeter size cantilevers operated in the dynamic flexural mode exhibit good sensitivities to gas mass density [7], [8], liquid mass density [9] and/or viscosity [10], [11].

With a view toward chemical detection in gas media, the variation of the gas density can reflect the variation of a chemical species concentration in a gas mixture [8], [12], [13], [14]. The operating principle of an uncoated silicon microcantilever (USMC) used as a density or chemical sensor is based on the influence of the mass of the fluid moved by the vibrating cantilever on the resonant frequency. In fact, when the surrounding fluid mass density increases (decreases), the equivalent effective mass of the cantilever increases (decreases), thereby causing the resonant frequency to decrease (increase) [12].

The absence of a coating eliminates or significantly reduces several problems associated with microcantilever-based sensors such as long-time response, drift and aging effects. However, uncoated microcantilevers are non-selective and offer very low sensitivities, making it quite challenging to detect small concentration changes (small density changes). This last point serves as the motivation to increase the sensor sensitivity through geometry optimization.

In the literature geometry optimization has already been reported for other particular cases of chemical detectors. For example, in the static bending mode, Loui et al. [15] have studied the influence of the length-to-width aspect ratio on the sensitivity of rectangular cantilevers due to both surface stress and an end-force loading. They have found that structures with a low aspect ratio are better for surface-stress applications and structures with high aspect ratio are optimal for point-loading scenarios. In the case of dynamic mode operation, the cantilever mass sensitivity is proportional to its resonant frequency. The resonant frequency is proportional to the square root of the stiffness and inversely proportional to the square root of the effective mass. Therefore, the majority of the studies conducted in order to improve the mass sensitivity of cantilevers are focusing on increasing the stiffness (k) and/or decreasing the effective mass (meff) using different methods. Hocheng et al. [16] have demonstrated using different microcantilever shapes that the higher the structural stiffness is, the better the sensitivity is. Similarly, Subramanian et al. [17] suggested the use of a nonlinear width profile for V-shaped microcantilevers in order to increase the structural stiffness and subsequently the mass sensitivity. For bio-sensing applications and in order to improve the overall (static-mode and dynamic-mode) sensitivity of a microcantilever, as measured by the product of static deflection and resonant frequency, Ansari et al. [18] proposed using a non-uniform cantilever cross-section (giving increased k and decreased meff) and reducing the fixed-end area (increasing the static deflection). The authors suggested triangular or step cross-section profiles instead the conventional rectangular one. Another solution, proposed by Narducci et al. [19], consisted of reducing the microcantilever size (increasing k and reducing meff) and/or using higher-order modes. In the case of end-mass loading, Morshed et al. [20] have demonstrated via simulation studies that structures with high aspect ratio (length-to-width) are more sensitive to local end-mass variation; furthermore, they have suggested the use of a triangular microcantilever shape to enhance the stiffness and minimize the effective mass at the free-end of the structure. Furthermore, to enhance the capabilities of microcantilevers in liquid media, Beardslee et al. [21] have studied the influence of the beam geometry on both the quality factor and the resonant frequency in a liquid medium (water) in order to limit the viscous damping effect, thus improving the detection limit of chemical sensing. The authors reported that the use of the in-plane bending mode reduces the damping and the mass loading due to the surrounding fluid, and that beams that are wide, thin and short and operated in the in-plane mode are more suitable for liquid-phase chemical detection.

As reported above, the resonant frequency is a key parameter in determining the cantilever mass sensitivity and all researches are focusing on enhancing this parameter. The microcantilever operating in fluidic (gas or liquid) environments interacts with the surrounding fluid which causes a distributed mass depending on the fluid properties, frequency and cantilever width [22]. Thus, although the resonant frequency is an important parameter to mass density sensing, the structure's geometry and dimensions play an important role in the mass density sensitivity of microstructures. In the present work we study the effect of microcantilever shape (rectangular, U- and T-shaped microstructures) and geometrical dimensions on the gas mass density sensitivity (i.e., the ratio of resonant frequency variation to the density variation). To perform this study several uncoated silicon microcantilever shapes with different dimensions have been designed and fabricated. The structures have been tested at room conditions using different concentrations (0.2–2.0%) of hydrogen (H2) in nitrogen (N2). The density changes have been measured by monitoring the eigenfrequency (natural frequency) variation using the efficient phase linearization method [23].

Section snippets

Modeling

The Euler–Bernoulli equation taking into account the hydrodynamic force acting on the uncoated microcantilever is commonly used to model the behavior of resonating microcantilevers in fluid media when the influence of the beam's shearing deformation and rotational inertia can be neglected [8], [12]. Fig. 1 displays the out-of-plane cantilever flexural mode (w is the free-end transverse deflection) and the geometric parameters: length (L), width (b) and thickness (h).

In this work, the

Experiments

In order to experimentally study the optimization of the sensor sensitivity, several microcantilevers with different geometries (rectangular-, U- and T-shaped microstructures) and dimensions (L, b and h) have been fabricated (Fig. 2b; Table 1) with electromagnetic actuation and piezoresistive read-out (Fig. 2a).

A gas line [23] has been used to generate different concentrations of H2 in N2 and to control the gas mixture flow. The different gas densities (ρH2N2), gas density variations (ΔρH2N2)

Experiment set #1: influence of the shape

This first experiment set was used for the first step of the sensitivity study consisting of the examination of the shape influence (rectangular-, T- or U-shaped structure) on the sensitivity. Fig. 4a and b shows the experimental measurements (markers) and the fitting lines of the first-mode natural frequency variation as a function of H2 in N2 concentration and density variation, respectively. The A2_5μ structure has the highest sensitivity (slope) among all of the other structures considered,

Conclusions

We have demonstrated that uniform rectangular cantilevers are more suitable for density measurement than the other tested T- and U-shapes. Moreover, wide and short beams are more sensitive to the density variation, with the sensitivity of the rectangular beams being proportional to b/L2. Furthermore, the thickness does not affect the sensitivity of rectangular cantilevers to the mass density changes despite the fact that it affects the resonant frequency. However, the noise on the resonant

Acknowledgment

The authors gratefully acknowledge the French National Radioactive Waste Management Agency (Andra, F-92298 Châtenay-Malabry, France. http://www.andra.fr/) for their support of this research. Grant number: UBX-Andra 055221 collaboration agreement.

Mohand-Tayeb Boudjiet received in 2012 the Master's degree in embedded electronics systems from University of Bordeaux in France. He is currently a Ph.D. student at IMS Laboratory working on microcantilevers for density measurement and chemical detection.

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    Mohand-Tayeb Boudjiet received in 2012 the Master's degree in embedded electronics systems from University of Bordeaux in France. He is currently a Ph.D. student at IMS Laboratory working on microcantilevers for density measurement and chemical detection.

    Johan Bertrand received in 2005 the M.S. degree in solid and inorganic chemistry from Rennes 1 University, France. In 2009, he earned his Ph.D. degree in physics and chemistry from the University of Tubingen and École des Mines de Saint-Étienne. Since 2009, he works for the National Radioactive Waste Management Agency as a Research Engineer on the development of an overall monitoring strategy and sensors development for the deep geological disposal of high-level and long-lived radioactive waste.

    Fabrice Mathieu was born in Orléans, France, in 1972. He received the Engineer degree in communication systems and electronics from the CNAM (Conservatoire National des Arts et Métiers), Toulouse, France, in 2003. He joined the Laboratoire d’Analyse et d’Architecture des Systèmes (LAAS), Center National de la Recherche Scientifique (CNRS), Toulouse, in 2001, where he is currently in charge of the development and the design of very low signal detection systems applied to the micro(nano)electromechanical systems area and its complete electronic treatment and control for automation.

    Liviu Nicu was born in 1973 in Bucharest (Romania). After completing his Master of Electrical Engineering at the Paul Sabatier University of Toulouse (France) in 1997, he joined the Integrated Microsystems Group at the LAAS (Laboratory for Analysis and Architecture of Systems) of Toulouse where he obtained his Ph.D. in 2000 into the Micromechanical Structures field. From 2000 to 2003, he was R&D Engineer at Thales Avionics, Valence (France). His activities focused onto the development of micromechanical sensors for the civil and military navigation applications. Since 2003 he joined the NanoBioSytems Group at LAAS as a full time CNRS (National Center of Scientific Research) researcher where he currently works in two main research fields: the development of (1) new resonant bio(chemical)sensors using M(N)EMS technologies and of (2) cantilever-based microsystems for contact deposition of small amounts of biological samples for biochip applications.

    Laurent Mazenq was born on May 30, 1982. He received his University Institute of Technology's Degree from the University Paul Sabatier de Toulouse (France) in 2002. Then, he joined the Laboratoire d’Analyse et d’Architecture des Systèmes of the French Center National de la Recherche Scientifique (LAAS-CNRS) as an Engineer Assistant. In 2011, he joined Freescale Semiconductor (France) in production process Engineering. He is working on UV projection lithography.

    Thierry Leïchlé is a CNRS researcher at the Laboratory for Analysis and Architecture of Systems in Toulouse (France). He obtained his M.S. from the Georgia Institute of Technology, Atlanta (USA), in 2002 and his Ph.D. from the University of Toulouse III in 2006. From 2007 to 2009 he was a postdoctoral fellow at the Institute of Physics, Academia Sinica, Taipei (Taiwan).

    Stephen M. Heinrich earned his B.S. from Penn State in 1980 and his M.S. and Ph.D. degrees from the University of Illinois in 1982 and 1985, all in civil engineering. He then joined the faculty at Marquette University where he is currently Professor of Civil Engineering. Dr. Heinrich's research has focused on structural mechanics applications in microelectronics packaging and the development of new analytical models for predicting/enhancing the performance of cantilever-based chemical sensors. The work performed by Dr. Heinrich and his colleagues has resulted in over 100 publications/presentations and three best-paper awards from IEEE and ASME.

    Claude Pellet was a researcher at the “Institut d‘Electronique Fondamentale” from the University of Paris XI-Orsay, where he studied the deposition of thin films by ion beam sputtering from 1982 to 1993. He joined University of Bordeaux as a full professor in 1993. His work focuses on micro-technology, micro-system development (humidity sensors), assembly technology and micro-systems reliability. He is currently the director of the IMS Laboratory, overseeing a staff of 400 people.

    Isabelle Dufour graduated from Ecole Normale Supérieure de Cachan in 1990 and received the Ph.D. and H.D.R. degrees in engineering science from the University of Paris-Sud, Orsay, France, in 1993 and 2000, respectively. She was a CNRS research fellow from 1994 to 2007, first in Cachan working on the modeling of electrostatic actuators (micromotors, micropumps) and then after 2000 in Bordeaux working on microcantilever-based chemical sensors. She is currently Professor of electrical engineering at the University of Bordeaux and her research interests are in the areas of microcantilever-based sensors for chemical detection, rheological measurements, materials characterization and energy harvesting.

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