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1-Port and 2-Port SAW Vapour Sensors 2006
1-Port and 2-Port SAW Vapour Sensors 2006
Received 2 December 2004; received in revised form 27 May 2005; accepted 30 May 2005
Available online 21 July 2005
Abstract
This paper reports an experimental study on chemical sensitivity and noise behavior of Colpitt and Pierce SAW oscillators based on
433.92 MHz one-port and two-port SAW resonator devices, respectively. The oscillators are characterized for phase noise as well as Allan
variance. The sensitivity for DMMP (di-methyl methyl phosphonate) vapor is imparted by providing a diallyl-bisphenol polymer precursor
as a selective interface coated on to both the SAW devices in an identical manner. Comparative vapor sensing experiments are carried out
under simultaneous exposure to the same DMMP vapor stream in different ranges of vapor concentration and duration. A new data acquisition
method is employed which is wireless and automated. It uses an antenna pickup at the input of a spectrum analyzer with PC control interface.
The results show that the two-port Pierce oscillator is more stable but less sensitive than the one-port Colpitt oscillator. It is found that under
the conditions of analyte exposure durations longer than 30 s the one-port Colpitt oscillator yields higher signal to noise ratios. The results
are interpreted in terms of phase response characteristics and different sensitivities of the one-port and two-port SAW devices towards mass
loading and viscoelastic effects.
© 2005 Elsevier B.V. All rights reserved.
Keywords: SAW oscillator; DMMP sensor; Phase noise; Allan variance; Mass and viscoelastic loading
0925-4005/$ – see front matter © 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2005.05.021
A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325 317
Fig. 4. SSB phase noise spectrum of the one-port Colpitt and two-port Pierce
oscillators used in this study.
Fig. 3. Phase slope of the two-port and one-port SAW resonators derived Fig. 5. Allan variance plot of the same two oscillators as shown in Fig. 4.
from phase responses shown in Fig. 2. The shaded area shows the spread of measurements.
A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325 319
Table 1
Different noise components and their regions of influence in 434 MHz TPP and OPC oscillators based on phase noise and Allan variance measurements in
Figs. 4 and 5
Noise component Dependence TPP oscillator OPC oscillator
SSB phase noise Allan variance SSB phase noise Allan variance
Offset frequency (Hz) Gate time (s) Offset frequency (Hz) Gate time (s)
White phase f0 20 k–1 M 34 k–1 M
Flicker phase f −1 τ −1 6–20 k
0.0001–0.1
9–34 k
0.0001–0.02
White frequency f −2 τ −1/2 2–6 k 7–9 k
0.1–1 0.02–8
Flicker frequency f −3 τ0 10–2 k 10–7 k
Random walk and aging f −n , n ≈ 4 τ n , n ≥ 1/2 1–10 1–200 1–10 8–300
offset frequency scale, which overlaps with the frequency transparent viscous liquid. It has been found to be stable for
region mentioned above in Fig. 4. The portions of phase more than 2 years. The device surfaces were plasma cleaned
noise spectrum above 10 kHz and Allan variance spectrum for 30 min to remove surface contaminants and to improve
below 1 s do not have mutually reciprocating information in the film adhesion and uniformity. A plasma cleaner system
Figs. 4 and 5. Therefore, the results of both measurements Roth & Rau AK350 with Ar ion plasma was used for this
taken together provide complimentary information about purpose. The freshly cleaned devices are then coated with
the behavior of the oscillators. Table 1 presents a summary the polymer dissolved in methanol by a drop dry method.
of these characteristics in terms of different noise types and Several other organic solvents such as dichloromethane,
regions of their performance. These values are obtained carbon tetrachloride, acetone and benzene were also tried.
by smoothening the phase noise curves after removing the With them, however, the deposits were always discontinuous
spikes and then by fitting to corresponding straight lines. The and comprising mostly globular/droplet like structure as
frequency range values in log scale have up to 3% errors. A shown typically in Fig. 6. The methanol solution produced
similar fitting is done for Allan variance measurements also. a smooth and continuous film with no visible feature when
The gate time range values in log scale have up to 12% error. examined under an optical microscope up to 80X. The poly-
It is not possible to differentiate between the white phase mer to solvent ratio was 1 mg/100 ml. The amount dispensed
noise and flicker phase noise since they both have the same was at 0.3 l/mm2 (optimized beforehand by independent
slope τ −1 [12]. experiments). The solution was dropped to cover the entire
Transitions between different regions are not clear. How- surface of the device without spilling along periphery. After
ever one can demarcate three regions as indicated in Fig. 5. visible evaporation of methanol the coated devices were
In the context of SAW sensor applications these regions can baked at 90 ◦ C for 5 h in a dry nitrogen ambience. This
be referred to as short term, medium term and long term resulted in an estimated film thickness of 3 nm.
stability regions. The significance of these regions depends The coated devices were then soldered to the oscillator
on the signal frequencies and associated readout times. For pcb. A sensor cell was then attached to the PCB as shown
instance, for ∼1 s readout time the TPP oscillator offers in Fig. 7. The sensor cell is made of stainless steel with two
nearly one order of magnitude higher frequency stability, holes for the two devices. The cell sits on the PCB with the
Fig. 5. However, the OPC oscillator may prove better in case
of low signal frequencies (<0.1 Hz, in the long-term region).
This is unlikely to be of much significance in SAW sensors,
which typically involve higher frequency signals. Owing to
the wider τ 0 region however the OPC oscillator exhibits fairly
constant stability over wide dynamic range of signal varia-
tions. This may result in more robust sensor performance.
Fig. 8. Schematic of the vapor generator/delivery system used for the char-
acterization of SAW sensors. V1 and V2 are two-port solenoid valves and
V3 is a three-port solenoid valve. M1 and M2 are flow meter and controllers. Fig. 9. Schematic of the data acquisition setup.
A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325 321
cell is used for the two sensors the sensing conditions are
identical. The inlet and outlet ports of the sensor cell can
be interchanged; and such an interchange produced the same
result. The vapor delivery system is made to pass the carrier
gas over the devices. The sensor oscillators are switched on
and allowed to stabilize for about an hour. The antenna is
placed as close as possible to the sensor oscillators to obtain
adequate signal power for the automated measurement. Data
acquisition software is run to record the oscillator frequen-
cies. The time taken for a measurement was ∼2 s and one
set of reading from both the oscillators takes ∼4 s. The ‘On’
(test + carrier gas passage over the sensor) and ‘Off’ (only
carrier gas passage over the sensor) durations are set on the
control circuit of the vapor delivery system. The ‘Off’ dura-
tion is kept at least three times that of the ‘On’ duration for
any measurement cycle. The data is continuously captured
and stored for analysis.
6.2. Observations
6.1. Setup
Fig. 11. Responses of the TPP and OPC sensor oscillators for simultaneous
The sensor cell is connected to the vapor generator keep- exposure to DMMP vapors in dry nitrogen at 250 ml/min, and for exposure
ing minimum distance between the two. Since a single small durations as indicated.
322 A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325
Fig. 13. Rise profiles of the TPP sensor upon exposure to DMMP test vapor
Fig. 12. The shift in frequencies of the TPP and OPC sensor oscillators normalized to the corresponding rise profiles of the OPC sensor for many
under identical DMMP exposure conditions for many continuous cycles cycles. The shaded area shows wide spread in the normalized values having
with exposure durations of 30 s, 60 s, 7 min, 20 min and 43 min. a general trend. Inset shows the averaged rise profile of many cycles and S/N
ratio crossover.
and OPC oscillator configurations under identical conditions
of experimentations. The low concentration of the analyte
tive time intervals. Though within 10 s of exposure though
vapor for long duration exposure cycles also avoids satura-
the average signal of TPP is seen higher than OPC, it can
tion of the sensors due to excessive loading.
be ignored as they lie within the error range of measurement
Fig. 12 shows the frequency shifts (signal) of the two oscil-
and normalization. The signal rise can be considered about
lators for several cycles of the different exposure durations.
the same for both the oscillators initially. For longer expo-
The reduction in magnitude of shifts with increasing time
sures, from the downward trend of the STPP /SOPC curve, it
(or cycle number) is due to reduction in vapor concentra-
is clear that the signal buildup in the OPC oscillator contin-
tion as the source slowly depletes with time. Shifts for single
ues while the TPP oscillator tends to stabilize (refer Fig. 11
cycles of long exposure durations of 7, 20 and 43 min at
also). Fig. 14 shows a similar ratio for the 43 min exposure
lower concentration are also shown in Fig. 12. Two points
duration (single cycle) at low concentration (∼0.1 ppm). The
are quite evident from these results: (i) the OPC oscillator
signal builds up faster in OPC oscillators than TPP oscillators
sensor generates nearly two times more shift compared to
up to nearly 200 s. Beyond 200 s the STPP /SOPC curve seems
the TPP oscillator for each exposure cycle of measurement.
to flatten, which means the buildup in both the oscillators
This means the sensitivity of the OPC oscillator is nearly
are the same. Beyond 1000 s, however, the STPP /SOPC curve
twice as high as the TPP oscillator for exposure durations of
shows an upward trend, though small, which means the sig-
at least 30 s and beyond; (ii) the fluctuation in signal level
nal in TPP oscillator is continuing to build up while the OPC
over several cycles of observation is also more for OPC than
oscillator is stabilizing. The presentation of data in ratios also
TPP. This is consistent with the Allan variance characteris-
eliminates uncertainty from lack of knowledge about precise
tics of the two oscillators reported in Section 2. From Fig. 5
vapor concentration.
one can notice that the Allan variance for the OPC oscilla-
tor is also about 2.5 times (on the average) that of the TPP
oscillator in the medium term region. This indicates that the
factors that are causing more fluctuations in OPC oscillators
are also responsible for generating more signals. Implicitly
these observations also suggest that the noise in both the oscil-
lators is limited by the SAW devices.
An interesting feature can be noted about the time depen-
dence of signal buildup in the two oscillators. Fig. 13 shows
the percentage ratio of the signal rise profiles of the two oscil-
lators for multiple cycles of 30 and 60 s exposure. This is
obtained by normalizing the frequency shift of TPP in the
‘On’ duration (STPP ) to that of the OPC oscillator (SOPC ) at
respective time intervals (i.e., STPP (t)/SOPC (t)%). The indi-
vidual fine traces in the shaded region correspond to different
cycles. The shaded area indicates the spread of such curves
and represents the approximate trend. The inset shows the Fig. 14. Rise profile of the TPP sensor for 43 min exposure to test DMMP
average of all the fine traces (normalized ratios) at respec- vapor normalized to the corresponding rise profile of the OPC sensor.
A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325 323
[7] J. Riebel, S. Stier, A. Voigt, M. Rapp, Influence of phase position University of Delhi, Delhi. He is working as a scientist at Solid State
on the performance of chemical sensors based on SAW device oscil- Physics Laboratory, Delhi since 1997. His present research interests are
lators, Anal. Chem. 70 (1998) 5190–5197. in SAW sensor systems and electronic noses, which include development
[8] Alexander Glas, Principles of SAWR stabilized oscillators, Applica- of low noise SAW oscillators, rf subsystem, digital subsystem (MCU,
tion note #1, Siemens Matshusita Components (Oct 1998) avail- PLD and FPGA) and sensor characterization. He has also worked in
able at http://www.web-ee.com/primers/files/saw-based oscillators the field of high TC superconducting thin films and transition edge
and transmitters.pdf. bolometer IR sensors during his PhD.
[9] D.E. Frerking, Crystal oscillator design and temperature compensa-
tion, Van Nostrand Reinhold Co., New York Library of Congress Mohan Singh was born in Bharatpur, India on August 2, 1972. He
card No. 77-17876, 1978 (Chapter 7). received his BTech in Electrical and Electronics Engineering in 1995
[10] W.L. Smith, T.E. Parker, in: E.A. Gerber, A. Ballato (Eds.), Precision from Birla Institute of Technology, Mesra, Ranchi. Presently he is work-
Frequency Control, vol. 2, Academic Press, London, 1985, pp. 53–61 ing as a scientist in Solid State Physics Laboratory, Delhi, since 2000.
(Chapter 8). Earlier he was working as a scientist in Defense Laboratory, Jodhpur
[11] RF 1172-433.92MHz SAW filter and RO 2101-433.92 MHz SAW (1997–2000). His main area of interest is in design and development of
resonator data sheets can be obtained from http://www.rfm.com of low phase noise SAW based oscillators for electronic noses and biosensors
rf monolithics Inc. and their characterization by Allan Variance, Phase Noise Measurement
[12] D.W. Allan, Time and frequency (time-domain) characterization, esti- and thermal modulation. He has also worked in high-resolution IR target
mation, and prediction of precision clocks and oscillators, IEEE development for defense applications.
Trans. Ultrason. Ferroelectr. Freq. Contr. 34 (6) (1987) 647–654. Upendra Mittal was born in Mathura, India in 1974. He received his BE
[13] P.K. Gutch, Vinita Dubey, G. Lal, D.K. Jaiswal, K. Shekar, Process (1997) from Institute of Engineers, Calcutta and ME (2003) in Electri-
for the preparation of an interface coating material for chemical cal Engineering from Delhi College of Engineering, University of Delhi.
sensors, Indian Patent, Application no. 265/DEL/2004. He is an Associate of Institution of Engineers (India), Calcutta. Since
[14] D.E. Tevault, J.H. Buchanan, L.C. Buettner, Ambient volatility of 1998 he is working in the area of SAW based chemical and biological
DMMP, in: Proceedings of the Fifteenth Symposium On Thermo- sensors in Solid State Physics Laboratory, Delhi. He has developed var-
physical Properties, Boulder, CO, USA, June 22–27, 2003. Available ious high stability SAW oscillator-based sensor prototypes. He is also
at http:/www.symp15.nist.gov/pdf/p440.pdf. involved in fabrication and characterization of SAW devices (filter, delay
[15] C.K. Campbell, Surface Acoustic Wave Devices for Mobile and line, resonator). His research interests are rf circuit design and rf char-
Wireless Communications, Academic Press, San Diego, 1998 (Chap- acterization. Currently he is working for the development of SAW based
ter 18). E-nose system.
[16] S. Martin, G.C. Frye, S.D. Senturia, Dynamics and response of
polymer coated surface acoustic wave devices: effect of viscoelastic R.D.S. Yadava received his BSc (Hons) (1974), MSc (1976) and PhD
properties and film resonance, Anal. Chem. 66 (1994) 2201–2219. (1981) in Physics from Benaras Hindu University, Varanasi. He is work-
ing as a scientist at Solid State Physics Laboratory, Delhi. His present
research interests include mainly the SAW devices and sensors, rf sig-
nal processing, pattern recognition and electronic nose. He has worked
Biographies in diverse research and development fields: SAW devices (filter, delay
line, resonator) design, fabrication and characterization, HgCdTe crystal
A.T. Nimal received his BSc (1991) and MSc (1993) in Physics preparation and characterization, IR detectors, MOS devices, fractals in
from Government Arts College, Bharathiar University, Coimbatore and noise and conduction phenomena, percolation systems, ion implantation
PhD (2004) in Physics from National Physical Laboratory, Delhi, and and radiation blistering in metals.