Thin-Film Piezoeelectric-on-Silicon Particle Mass Sensors Brandon P. Harrington and Reza Abddolvand Arash Hajjam, James C. Wilson, and Siavash Pourkam mali School of Electrical and Computer Enginneering Oklahoma State University Tulsa, OK, USA [email protected] University off Denver Denver, CO O, USA Abstract — In this paper, high quality factor (Qair>18000), high frequency (~27MHz and ~54MHz), lateral--extensional mode thin-film piezoelectric-on-silicon resonators arre used as aerosol particle mass sensors. Using an aerosol particcle generator, mass sensitivities of -4.2Hz/pg and -42Hz/pgg are measured respectively which confirms the benefits of employing higher frequency resonators given the quality factor iis not deteriorated. These results are in good agreement with th he theoretical and simulated values. Our work suggests the TPoS S resonators as an easily integrated, low-loss platform for particle sensing applications. I. INTRODUCTION make atmospheric Currently, the equipment required to m particle measurements are bulky and expennsive and do not provide desired levels of performance [1] [[2]. Atmospheric aerosol particles ranging in size from a few nm to tens of um have a direct impact on air quality and thhereby have a far reaching effect on health [3] and global clim mate [4]. MEMS resonators functioning as mass sensors can prrovide a low-cost, high-sensitivity, and easy to integrate platfforms for aerosol measurement instruments. MEMS resonatoors with their high frequencies and very small masses can achieve greater mass sensitivities. However, without addressingg the operational noise level, gain in sensitivity would not neccessarily yield in a better sensor. The resonator’s high mechaniical quality factor (Q) can work to improve the signal-to-noisee ratio (SNR) and therefore lower minimum detectable mass w while allowing low power operation. To date, many approaches to MEMS mass sensors have been investigated. Capacitive-transduced, very high-Q ((>100,000) mass sensors have been demonstrated in the paast. However, for capacitive devices to operate at high frequeency, very narrow transduction gaps are required [5]. For m mass sensing this small gap is undesirable. First the significcant gas damping forbids this type of device from operation in air with a high Q. Lastly, the small transduction gap providdes an additional failure mechanism by allowing particles trappped in the gap to obstruct the resonator’s motion. 978-1-4244-6401-2/10/$26.00 ©2010 IEEE Thermally actuated resonant masss sensors are a relatively new idea. They offer operation in atmospheric a environments and exhibit great robustness against deposition of contaminants and particulates on theeir structures [6]. On the other hand, their high power consum mption (tens of mW) could limit remote or portable use. Recently, nanomechanical resonaators have been pursued to push the minimum detectable mass liimits closer to single atom level. Such tiny resonators benefit from f their extremely small masses to achieve this performance.. However, these devices typically suffer from relatively lo ow quality factors, low resonant frequencies, and nanoscalee transduction challenges [7]. A thin-film piezoelectric-on-siliicon (TPoS) resonator as seen in Fig. 1, offers a unique solution in comparison to the previously mentioned approaches. In combination with the low loss single-crystal silicon reesonant body, the high piezoelectric transduction coefficientt results in a low motional impedance device. The TPoS resonaator design is able to scale its frequency into the GHz regime while w maintaining a high Q in air with little detriment [8]. Osciillators operating at 1GHz with low phase noise based on high h-Q TPoS resonators have already been realized in [9] so an exttension to high frequency, high-Q, low-noise mass sensing witth these devices is readily obtainable. Silicon Metal Electrode Piezoelectric Layer Ground Plane Via Figure 1: A 3rd order lateral extensional thin-ffilm piezoelectric-on-silicon resonator (TPoS). 238 THEORY In a resonant mass sensor, the incidennt mass particles perturb the measuring resonator through aadditional inertial mass causing the resonant peak to shift. If the resonator resides within an oscillator circuit, the reesulting oscillator frequency becomes dependent on the absorbeed mass. 0.994) mass sensitivity of in Fig. 2 has a nearly linear (R2=0 -43.9Hz/pg. 55.274 Frequency (MHz) II. To accurately analyze the mass sensinng limit for any resonator one must look at the different addittions of noise into the system. Fortunately much work has beenn done in this area showing the dominant source of noise to be thermomechanical fluctuations. When limited by thhis phenomenon, it has been shown that the minimum detectablee change in mass, (δM) in a PLL-based is [10]: ∆ 55.271 55.269 , (1) 0 where the Meff is the effective mass of the reesonator, Eth is the thermal energy, Ec is the maximum drive energy at critical vibration amplitude, Δf is the measurementt bandwidth, Q is the resonator quality factor, and ω0 is the aangular resonance frequency. The first ratio represents the inveerse of the signalto-noise ratio and shows that the more poweer is driven to the resonator while it remains linear, the smaller the detectable change in mass will be. In addition, if the measurement bandwidth is increased, the thermo-mechannical noise grows, lessening the sensitivity. The two most common approaches to reeducing δM are to make the device less massive (lower Meff) oor to increase the frequency-Q product (f.Q). Most approachees to mass sensing have been focused on the former, Meff reducttion. In doing so, these devices have been hampered by reduceed Q. The goal of the devices in this paper is to increase the ff.Q in an effort to improve the minimum detectable mass changge (δM) and mass sensitivity (δf/δM). Even so, in the effort to increase f.Q, tthe overall sensor performance can still be limited. A pushh to ever higher frequencies can lead to a diminished Q yet sstill a greater f.Q. Q has been shown to be inversely proportiional to the Allan deviation, the standard measure of short-term m instabilities [11]. Therefore, to truly improve the performancee for an oscillatorbased mass sensor, Q should remain constaant or improve as the resonant frequency increases. Sincce current TPoS resonator f.Q of 6.6x1012 [9] have not approached the maximum theoretical f.Q for the single-crystaal silicon resonant structure, 1014 as predicted by [122], simultaneous improvement in frequency and quality factor is still obtainable. III. 55.272 55.270 IV. 40 0 Number of Particles P 60 80 RESONATOR DESIGN AND A FABRICATION To study the effectiveness of the t resonators as a mass sensor, 27MHz and 54MHz reson nators were designed and fabricated. The resonators were fabricated f on 30μm thick device layer SOI wafers with a piezo oelectric aluminum nitride layer, sandwiched between two moly ybdenum layers that form the electrodes and electrical interco onnects. The five mask procedure is a low temperature (< 250C), post-CMOS compatible process starting with thee layered stack on top of the SOI wafer. After a series of o dry etches define the electrode shape and resonator body, the handle silicon layer is anisotropically wet etched from the backside stopping at the SOI buried oxide layer. The reson nators are released with a wet etch to remove the exposed ox xide layer. The complete fabrication process has been descrribed in detail previously [13]. SEM images of fabricated devices are shown in Fig. 3 d with 27MHz and and 4. Prior to testing, the two devices 54MHz resonant frequencies weree tested in air using a network analyzer; their frequency responses are seen in Fig. 3 and 4 respectively. 0 Air Operation f0 = 27.37MHz Qunloaded = 23000 Rm = 262Ω mass = 3.09μg -20 SIMULATION To evaluate the TPoS mass sensorr’s sensitivity, a COMSOL Multiphysics structural mechannics simulation is utilized. The eigen-frequencies of a single-ccrystal silicon slab of dimensions 114.8μm by 76.5μm by 30μm m with no support tethers or loss mechanisms are examined. O One micron cubic nylon particles are randomly distributed acrross the sensor to imitate deposited aerosol particles. The frequency of the targeted mode shifts as a response to tthe added mass. Through 75 particles, a simulated 54MHz maass sensor as seen 20 Figure 2: Simulated frequency shift from added a particles on a 54MHz mass sensor. A meshed single-crystal silicon slab with eight particles wn in the top right. randomly distributed on the surface is show |S12| (dB) 2 55.273 -40 -60 -80 27 28 29 Frequency (MHz) ( Figure 3: SEM image and frequency responsse for a fabricated 27MHz TPoS resonator. 239 25 26 VI. -20 Aiir Operation f0 = 53.99MHz Quunloaded = 19000 Rm = 3.8kΩ m mass = 0.63μg As expected, the frequency decrreases linearly due to the additional mass loading as the partiicles are deposited on the device, (Fig 6). The frequency respo onses show an increase in loss and therefore motional impeedance as more mass is deposited (Fig. 7). -60 Frequency(MHz) -80 -100 50 52 54 56 58 Frequency (MHz) Figure 4: SEM image and frequency response for a ffabricated 54MHz TPoS resonator. V. 27.2908 53.8925 27.2906 53.8920 53.8915 27.2904 53.8910 27.2902 53.8905 27.2900 53.8900 27.2898 53.8895 27.2896 53.8890 Frequency (MHz) |S12| (dB) -40 RESUL LTS 0 20 40 Time(min) Figure 6: Change in frequency as aerosol-d dispersed particles are deposited on the 27MHz and 54MHz reson nators CHARACTERIZATION N An aerosol particle generator, shown in F Fig. 5, was used to deposit particles with known size (and thereffore known mass) onto the fabricated resonators. To form uniiform particles, in the particle generator atomized droplets of m methylene blue in ethanol are pumped through a Kr-85 biipolar charger to establish a near Boltzmann charge distributioon centered at zero charge for the droplets. As the solvent driies, the remaining solid spherical aerosol particles are injecteed into a column with a large electrostatic field which defl flects the moving charged particles based on their mass andd charge. In this manner particles are separated based on thheir mass and the specific desired diameter, nominally 1μm m for the tests discussed in this paper, is selected. -59 -61 dB -63 10m 0m 20m 30m -65 -67 -69 -71 -73 53.885 53.887 53.889 53.891 53.893 5 53.895 53.897 Frequency (M MHz) Figure 7: Frequency responses through tim me as more particles are collected on the resonator. The high loss (relative to the meaasured frequency response of Fig. 4) seen in the captured data of Fig. 7 is attributed to the d to make the particle vacuum interconnections required measurements. SEM images of the 27MHz device after testing can be seen in Fig. 8. Using this image, the number of p and therefore particles are counted (~330 particles) approximation for the mass depositeed on the sensor (Mp) can be calculated using (2) Figure 5: Aerosol particle generator with the capabiliity to select outgoing particle size Particles are propelled and deposited onn the device under test in a low vacuum environment (~50-1100Torr) inside a glass bell jar. The device which has been wire-bonded to a PCB is mounted in the tool and attached to a network analyzer through vacuum feedthroughs. Prior to deposition, the particle nozzle is aligned over the target device using a microscope and a micropositioning stage. Frequenccy spectrums are captured at regular intervals through the depoosition. where N is the number of particlees, D is the approximate diameter, and ρ is the density of thee aerosol particle resulting in a calculated mass of 213pg. Likeewise, the same procedure was performed on the 54MHz device (Fig. 9) resulting in 110 particles or a calculated mass of 70.8pg. The overall frequency shifts seen in Fig. 6 are -904.5Hz and -296.3Hz for the 27MHz and 54MHz resonators respectively. nsitivity for the 27MHz is Therefore, the experimental mass sen found to be -4.2Hz/pg while that of o the 54MHz design is 41.9Hz/pg, a tenfold improvementt. The increase can be attributed to the double in operating frequency and a five times reduction in structural mass. 240 VII. CONCLUSSIONS The thin-film piezoelectric-on-siilicon (TPoS) based mass sensors shown in this paper offer low motional impedance (<3kΩ), high Q (>18000), and high frequency (27MHz) with mass resolution up to -4.2Hz/pg show wn in this work. Through doubling the frequency to 54MHz wh hile maintaining a high Q, the TPoS mass sensor shows roughlly a 75% reduction in the minimum detectable mass and a teen times improvement (41.8Hz/pg) in experimental mass sensitivity s while agreeing well with theoretical and simulated d results. The completed device has been shown to operate in air making the sensor function with less power and in moree lenient packaging. Figure 8: SEM image of the 27MHz mass sensor afteer exposure to aerosol particles. This device has ~330 particles on it. VIII. REFEREN NCES [1] [2] [3] Figure 9: SEM image of 54 MHz mass sensor after exxposure to aerosol particles. This device has ~110 particles on it. Assuming the resonator’s compliance remains constant during the deposition, the deposited mass ccan be calculated using [4] [5] (3) where ∆f0 is the change in frequency, f0 is the resonant frequency, ∆Meff is the change in mass, and Meff is the effective mass of the resonator [11]. Since thhe deposited mass is small and not affecting the mode shape, tthe mass ratio can be written as the change in mass divided by total effective mass. With (3), the expected mass depositeed on the 27MHz resonator calculated from the -904.5Hz shiift is found to be 205pg, with a 3.6% error. For the 54MHz reesonator, -2963Hz frequency shift translates into the expectedd mass of 69.2pg, resulting in a theoretical error of ~2.3% and a simulation error of ~5%. To estimate the ratio of minimum detectable mass (δM54MHz/ δM27MHz) using (1), the measureement bandwidth, Δf, and the thermal energy, Eth, can be assum med to be constant between the two mass sensors. The result, (4) where V is the volume of the resonator and < <x2> is the critical displacement amplitude, shows that increasinng f.Q will reduce the minimum detectable mass. 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