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Sensors and Actuators B 114 (2006) 316–325

A comparative analysis of one-port Colpitt and two-port


Pierce SAW oscillators for DMMP vapor sensing
A.T. Nimal ∗ , Mohan Singh, U. Mittal, R.D.S. Yadava
Solid State Physics Laboratory, Lucknow Road, Timarpur, Delhi 110054, India

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

1. Introduction the minimum level of an analyte that can be detected. The


sensor oscillators should be free of frequency drifts (during
Surface acoustic wave (SAW) chemical sensors employ at least the measurement duration) in order to differentiate
polymer coated SAW devices as frequency control elements the chemical signal from any spurious frequency shift. The
in oscillator circuits. These are rf oscillators operating at stability should be high so as to achieve high signal to noise
frequencies in the range of few MHz to about a GHz. They ratio, which would lead to low detection limits. The dynamic
work on the principle of mass loading and are highly sensitive range depends upon the mass sensitivity as well as the range
to minute quantities of chemical analyte loading on the SAW over which the oscillator can be pulled from its operating
propagation path. The shift in SAW velocity due to surface point. The improvement of the sensitivity is achieved
loading leads to a shift in phase, which in turn generates a shift through innovations on the adsorbent coating [1,2], increas-
in frequency of the oscillator. This shift in frequency under ing the frequency of operation [3] and device characteristics
analyte exposure is the sensor signal. Important features [4–6].
that define the performance of these sensors are selectivity, All these characteristics however cannot be optimized
sensitivity, stability, response time and dynamic range. The independently, and several trade-offs are needed. The sta-
selectivity for a target analyte depends solely on the polymer bility can be improved by using SAW devices with high Q
coating. The sensitivity along with the stability determines factors, but this will compromise the dynamic range due to
low oscillator pullability (narrow bandwidth of operation).
∗ Corresponding author. Tel.: +91 011 23960609; fax: +91 011 23913609. Improvement in sensitivity can also be achieved through
E-mail address: atnimal@yahoo.com (A.T. Nimal). improvisations in oscillator designs. Riebel et al. [7] have

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

recently reported improvement of sensitivity by tuning the


phase point of oscillation in the pass band of a sensing SAW
resonator device. The fast sensor response would be obtained
through weak vapor–polymer interactions, but this will also
result in poor sensitivity. In the present paper we report on the
construction and behavior of two different oscillator config-
urations (Colpitt and Pierce) using 434 MHz SAW resonator
(one-port and two-port) devices. The oscillators are compared
for their stability in both the frequency and time domains.
Their performance towards sensitivity for DMMP (di-methyl
methyl phosphonate) analyte vapor is compared by coating a
diallyl-bisphenol polymer precursor on both oscillators under
identical conditions. This study aims at analyzing the rela-
tion between stability and sensitivity of SAW vapor sensors
based on one-port and two-port resonator devices, and seeks
optimum conditions of operation that can result in the lowest
level of detection.

2. Construction and characterization of SAW


oscillators

The 434 MHz SAW resonator devices used in this study


were obtained from RF Monlithics. The one port SAW
resonator RO2101 is used for making a common base Colpitt
oscillator and the two port SAW resonator RF1172 is used for
making a Pierce oscillator [8]. Hereafter, the two oscillators
will be referred to as OPC (One Port Colpitt) and TPP (Two
Port Pierce) oscillators. Fig. 1 shows the circuit used for real-
izing these oscillators. Single stage rf transistor amplifiers
have been used. The design uses surface mount components,
and both the oscillators operate at 3 V power supply. The
SAW devices in TO-39 package are inserted from one side of
the PCB (Printed Circuit Board) so that the solder pins appear
on the opposite side where all other electronic components
are placed. The two oscillators are placed closely on a single
PCB so as to accommodate the two sensor devices in a single
sensor cell with a minimum dead volume. Tuning of the Fig. 1. Schematic circuit diagram of (a) a pierce oscillator with two-port
inductances and capacitors are crucial for the operation of SAW resonator (TPSR) and (b) a colpitt oscillator with one-port SAW res-
these oscillators. In the OPC oscillator, the tank circuit LC , onator (OPSR) devices at 433.92 MHz.
C1 and C2 are fine tuned by placing a short at the location of
the SAW device. Once the frequency of oscillation is brought provide the remaining phase shift to make it 360◦ . The phase-
close to that of the SAW resonator, the short is replaced by loop condition is satisfied by the two-port SAW device and
the device. In case of the TPP oscillator the device is placed the two tuning inductors L1 and L2 . The shunt elements here
in the feedback loop and fine-tuning of the feedback network are the IDT capacitances and other parasitic capacitances. For
is carried out. The outputs of the oscillators are monitored by this feedback network to operate successfully it is required
using a spectrum analyzer, an oscilloscope and a frequency that the reactance of series elements and the shunt elements
counter. have opposite signs. The SAW device is forced to operate
In general, the Pierce oscillator configuration is more in the positive reactance condition assuring the maximum
stable than the Colpitt [9,10]. The two configurations used phase slope. These aspects are discussed in detail in Section
in this study have different features that lead to variations in 8.1.2.2 of reference [10]. In the OPC oscillator, Fig. 1(b),
their stability or noise figures. In the TPP oscillator, Fig. 1(a), the tuning network in the collector circuit effectively limits
the two-port SAW device and the associated tuning network the bandwidth of the oscillator. The transfer phase of the
form the band pass phase inverting feedback network. The common base stage remains near zero. The impedance
transfer phase of the transistor is ideally 180◦ (practically presented to the SAW branch by the emitter is relatively
exceeds this value) and the feedback filter network must low and hence the phase slope of the feedback network is
318 A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325

Fig. 4. SSB phase noise spectrum of the one-port Colpitt and two-port Pierce
oscillators used in this study.

the two-port device used in the TPP oscillator has a larger


phase slope. This results in the higher oscillator stability.
The phase noise and Allan variance measurements of the two
Fig. 2. Frequency and phase response of the one-port and two-port oscillators are shown in Figs. 4 and 5, respectively. The phase
433.92 MHz SAW resonators. noise measurements were done by using the Aeroflex PN9000
setup. The measurements were performed in the phase lock-
not seriously degraded. In contrast to the TPP oscillator, the
ing mode using Hanning window. Stable dc power supply
SAW device in the OPC oscillator is not a resonant network,
for the oscillators is obtained from Agilent model E3620A.
and therefore does not carry circulating currents.
The Allan variance measurements were performed by using
The stability or noise figures of these oscillators also
Fluke PM6681 timer counter and ‘Time View’ software. The
depend on the phase characteristics of the SAW devices used.
‘Time View’ is a statistical data collection and analysis soft-
The measured amplitude and phase response of the devices
ware. The oscillators were powered on and allowed to warm
used in this study are shown in Fig. 2. The one-port resonator
up for a minimum period of 1 h before taking measurements.
used in the OPC circuit has a single amplitude transfer peak
The phase noise behavior of the two SAW oscillators
and the oscillation is setup close to it. The two-port device
shown in Fig. 4 is consistent with the Allan variance charac-
used in the TPP oscillator has two peaks close to each other.
teristics in Fig. 5. It can be seen that the phase noise of the
No external matching networks are used here. However, this
TPP oscillator is consistently lower than the OPC oscillator
device with a proper matching network is reported to be a
in the measured offset range from 1 Hz to 200 kHz. A similar
filter with a single 600 kHz pass-band [11]. To realize oscil-
trend can be noted for the Allan variance as well in Fig. 5
lator operation with this device the first frequency peak is
over the range of measurement durations from 0.1 ms to 5 s.
used where the insertion loss is minimal. The phase slopes
This range of duration corresponds to 0.2 Hz to 10 kHz on the
−dφ/dω of these devices are shown in Fig. 3. It is clear that

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.

3. Polymer coating and sensor packaging

The devices in TO-39 package were cut open in order


to gain access to the device surface. The DMMP-selective
material was coated on the SAW devices to make them
sensors. The material used is a diallyl-bisphenol polymer
precursor, which is hydrogen-bond acidic and a structural tar-
get for many of the BSP hybrid organic-inorganic polymers Fig. 6. A typical optical micrograph of the polymer deposited on ST-quartz
[13]. This material has earlier been evaluated as a stationary crystal surface by dissolving it in dichloromethane. The arrows demarcate
phase for gas chromatography. It is a slightly brownish, the drop boundary.
320 A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325

When one path is closed the corresponding two-way vent


valve (V1 , V2 ) is opened simultaneously to vent out gases.
Fast switching solenoid valves operated by microcontroller-
based electronic control circuits are used in this system. This
ensures continuous flow of gases along the two paths with
negligible flow disturbance during switching of the solenoids.
When the test gas is passed to the sensor it is considered as
‘On’ state and when the carrier is passed it is ‘Off’ state. The
‘On/Off’ durations can be set as desired. The complete vapor
Fig. 7. Schematic of the sensor cell fitted to PCB which can accommodate
two SAW sensors and has minimum dead volume. generation and delivery system is kept at room temperature.
This arrangement gives reasonably stable DMMP vapor
two open devices inside the cell. Care is taken to avoid strain concentration till the source liquid is present in the container.
on PCB due to the placement of the cell. Teflon and silicone Depending on the DMMP liquid load stable vapor concen-
rubber ‘O’ rings are used to seal the cell. The inlet and outlet tration condition was obtained from a few minutes to nearly
of the cell are designed such that the gas does not hit the an hour for different experiments. When the volatile liquid is
devices directly. The design of the cell is such that the dead taken in very small quantities the vapor concentration keeps
volume is minimized. decreasing with time until finally the liquid completely evap-
orates. This feature is advantageously used to examine the
sensor behavior over a wide range of analyte concentration.
4. Vapor generation and delivery system By taking larger quantities of the volatile liquid and main-
taining the quantity in the container it is possible to maintain
A laboratory-made vapor generation and delivery system the vapor concentration at a fixed level for reasonable
shown in Fig. 8 is used for carrying out DMMP sensing duration needed for various measurements. The maximum
experiments. Dry nitrogen is used as the carrier gas to carry DMMP vapor concentration under stable source condition
the test vapor to the sensor. A little quantity of the volatile was estimated to be ∼0.5 ppm. The estimation is based on
DMMP liquid is placed at the bottom of a corrugated glass DMMP vapor pressure data given in [14] (153 Pa at 300 K).
container, and the carrier gas is continuously passed through
headspace as shown. The liquid is loaded by using a syringe
inserted through the silicone rubber septum at the top of the 5. Wireless data acquisition using spectrum analyzer
container. Corrugations of the container facilitate mixing of
the carrier and analyte vapor. The carrier gas from the source The frequency data acquisition from the two sensors is car-
is bifurcated into two paths, controlled by individual flow ried out through a radiation pickup using a spectrum analyzer
controllers, one carrying the test gas and the other only the interfaced with PC, schematically shown in Fig. 9. A copper
carrier. The flow rates along the two paths are maintained at wire about the length of the wavelength of the oscillators
250 ml/min. The three-way solenoid valve V3 is used to open connected to an rf coaxial cable is used as an antenna. The
one of the two paths and its outlet is connected to the sensor. spectrum analyzer (HP 8591E) receives the radiation through
the antenna and displays the two frequency peaks. The fre-
quencies can be measured with high resolution by zooming
to the peak position and using “peak search” option. In this
method the oscillators are not loaded by the output network,
and needs for matching and/or amplification are avoided.
Moreover, mechanical strain on PCB due to connecting

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

When these sensor oscillators are simultaneously exposed


to the same DMMP vapor stream the frequencies of the
two oscillators decrease by different amounts. Fig. 11 shows
typical response cycles with the analyte exposure (‘On’) dura-
tions of 30 s, 60 s, 7 min, 20 min and 43 min. For these mea-
surements a small quantity of DMMP liquid was loaded at the
bottom of the source container (Fig. 8). The 30 and 60 s dura-
tion measurements were recorded at an early stage of analyte
vaporization when the vapor concentration is fairly stable.
Fig. 10. Flow diagram of the software written in VB to acquire data from
spectrum analyzer through GPIB.
The 7, 20 and 43 min observations correspond to the stage
when no trace of liquid is visible and only the remnant con-
tamination of the container produces low vapor concentration
shielded cables are avoided. Thus the oscillators are electri- (∼0.1 ppm). Though these concentrations are not precisely
cally independent of the measurement and data acquisition measured, it is immaterial in the present context as our inter-
system. During sensing experiments the frequencies change est is basically to compare the relative behavior of the TPP
fast, and therefore the measurements need to be faster. To
facilitate this, an IEEE 488 interface is setup between the
spectrum analyzer and a PC. Software written in Visual
Basic is used to acquire the data from the spectrum analyzer.
The program flow of the software is shown in Fig. 10. The
two frequencies are noted sequentially by zooming to their
positions for the maximum resolution. A drawback of this
type of acquisition is that the minimum interval between
two consecutive readings is about 2 s. However it is possible
to increase the speed of acquisition at the cost of resolution.
The frequency data in the present study were recorded with
resolution of 3 Hz. Note that this readout time corresponds to
the medium term stability region of the oscillators (Fig. 5).

6. DMMP sensing experiment

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

The fluctuations in the frequencies of the two oscillators


were monitored while exposing only to the carrier gas (‘Off’)
for long durations over several measurements. Similar to the
above, the fluctuations (or noise) in consecutive frequency
readings of TPP oscillators (NTPP ) are normalized to that
of the OPC oscillator (NOPC ) at respective time intervals
(i.e., NTPP (t)/NOPC (t)%). It is found that the average of these
noise ratios of the two oscillators over several measurement
cycles has a value of 68%. It is noted that the Allan variance
measurements reported in Section 2 were performed under
static conditions when no gas is flown over the device. The
fluctuations measured during passage of carrier gas over
the device includes additional noise due to factors like flow
rate, pressure and temperature. Therefore, the observation
that NTPP < NOPC implies that the OPC oscillator is more
Fig. 15. The representative phase curves of a one-port and a two-port device
susceptible to these spurious perturbations. Horizontal lines
before and after vapor loading simulated from the equivalent circuit of SAW
corresponding to this noise ratio of 68% shown in the inset resonators (inset).
of Fig. 13 and in Fig. 14 intersect the signal ratio curve
at about 30 and 50 s of exposure duration, respectively.
This shows that up to these exposure durations the S/N SAW resonator devices. Fig. 15 shows the equivalent circuit
ratio of the TPP oscillator is more than the OPC oscillator of SAW resonators along with representative phase curves of
(STPP /SOPC > NTPP /NOPC or STPP /NTPP > SOPC /NOPC or a one-port and a two-port device. Note that the equivalent cir-
(S/N)TPP > (S/N)OPC ) and beyond these durations it is cuit of the SAW resonator is consisted of a motional arm (LM ,
the reverse. The significance of these observations is CM , RM ) in parallel with a static arm (CO for one-port and
that the TPP oscillators are better suited for making fast CP for two-port) due to static IDT capacitances. For making
responding sensor systems involving small durations of sensor oscillators the static capacitances are either tuned out
analyte contact. However, the OPC oscillators can yield or made insignificant, and the oscillators are controlled by
a lower limit of detection if longer exposure durations the motional arm alone. Modification of an equivalent circuit
are employed. The choice of oscillator configuration and of the SAW resonator under vapor mass loading and polymer
analyte contact time depends on the concentration range viscosity has been studied in detail by Reibel et al. in [7].
of interest. Their model assumes that the adsorption of the vapor causes
increases in the inductance and resistance (or adds additional
inductance and resistance in series). Pure mass loading
7. Discussion appears as a change in motional inductance. The increase
of inductance causes the phase curves shift towards lower
The phase noise characteristics of both the oscillators can frequency, while the increase of resistance causes broadening
be explained in terms of the Leeson’s model as summarized or flattening of the phase curve. It is reported that the vapor
in [15]. The lower SSB phase noise of the TPP oscillator at adsorption with thin coating merely moves the phase curve
low offset frequencies (below 100 kHz) arises from the larger of the resonator towards lower frequency, whereas thick film
phase slope of the two-port resonator device in its control coating causes the phase curve to flatten also [7]. It should be
circuit compared to that of the one-port resonator device used noted that the polymer coatings used in our case are very thin
in OPC oscillator (Fig. 3). For a SAW resonator the quality and therefore the dominant change in the equivalent circuit
factor Q at the resonance is defined as Q = 1/2ω0 (−dφ/dω) would appear on the inductive part. Our observations on vapor
where ω0 denotes the angular frequency of resonance. The sensitivity can be explained by considering the phase curves
white frequency (f−2 ) and flicker frequency (f−3 ) noise in Fig. 15. The values of the motional components for the one-
components of a SAW resonator oscillator are inversely port SAW resonator device are obtained from the data sheet
proportional to (Q/ω0 )2 or (−dφ/dω)2 [15]. Therefore, [11] of the manufacturer. For the two-port SAW resonator
the TPP oscillator would obviously be less noisy, or more these values are calculated for the first peak by matching the
stable. In the f0 region beyond 20 kHz, however, both phase slope. The values of RI and RL were adjusted slightly
the spectra converge to the same floor level of nearly to match the measured phase slope and they were kept the
−142 dBc/Hz. According to equation (18.7) of reference same for both the devices. Parasitic capacitances are not
[15], this indicates that at higher offset frequencies both taken into account. The estimated value of inductance for
the oscillators are limited by the amplifier noise in the the two-port resonator is 3.16 times to that of one-port. The
circuit. dotted curves correspond to the case of vapor mass loading
The difference in mass sensitivity of the two oscillators causing an increase in inductance by ␦L = 20 nH. The phase
can also be explained in terms of the phase slopes of the curves of both the SAW devices are shifted towards the
324 A.T. Nimal et al. / Sensors and Actuators B 114 (2006) 316–325

lower frequency by different amounts. The one-port device 8. Conclusion


with a lower phase slope is shifted more. In order to maintain
the loop phase condition in oscillator configuration the In this study we find that the one-port SAW resonator-
frequency would decrease by 50 kHz for OPC and by 16 kHz based Colpitt oscillator makes a more sensitive chemical
for the TPP for the assumed change in LM . That is, the OPC sensor than the two-port SAW resonator-based Pierce oscil-
oscillator is more than three times more sensitive than the TPP lator. Even though the noise (SSB phase noise and Allan
oscillator. variance) for the Colpitt oscillator is more, this oscillator
From Figs. 12 and 13 we have seen that the OPC oscillator offers better S/N ratios for vapor exposure durations beyond
shows 2.5 times higher sensitivity than the TPP oscillator. A 30 s. It is concluded that this behavior is due to differences in
small increase in the resistance value of the motional arm in the phase slopes and the viscoelastic stiffening effects for the
the equivalent circuits can cause flattening of the phase slope one-port and two-port resonator devices. During initial stages
and lessen the effect. Also the reason for the observation that of vapor exposure the pure mass loading effect generates the
for longer durations of vapor exposure the OPC oscillators signal. At later stages when the analyte homogenization and
continue building up the signal and attain higher S/N ratios for polymer stiffening sets in the effect of mass loading is reduced
exposure durations beyond 30 s is not immediately obvious. due to the opposite sign of the viscoelastic effect. This cancel-
It can be explained in terms of the viscoelastic effects if (i) lation appears more effective in the two-port resonator device.
polymer stiffening becomes significant during the later part That means a two-port resonator device is more sensitive to
of vapor exposure, and (ii) the two oscillators have different viscoelastic effects. The differences in the mass sensitivity
sensitivities for this effect. As is known the sign of frequency and noise behavior of the two oscillators have been explained
shift due to viscoelastic stiffening is opposite to that due to the in terms of phase response characteristics. The higher phase
mass loading [16]. Therefore, for a given analyte exposure slope of the two-port device results in lower phase noise (or
the mass loading increases the signal and the viscoelastic better stability). However for the same reason the two-port
stiffening reduces it. Note that the viscoelastic effects will has poorer mass sensitivity. The one-port resonator device
appear at later stages of the exposure as it involves analyte has higher mass sensitivity and lower viscoelastic sensitivity.
homogenization in the polymer matrix following the initial This makes the one-port Colpitt oscillator to become a better
sorption in the top surface layer. It seems that the one-port sensor.
OPC oscillator is less sensitive to the viscoelastic loading than
the two-port TPP. If this is true then the mass loading effect
will be retarded more effectively in the TPP oscillator, and the Acknowledgements
saturation will set in earlier than that in the OPC oscillator.
At lower concentrations the time taken for the viscoelastic The authors are thankful to the Director, SSPL for his kind
effects to be appreciable is more, and thus the S/N crossover permission to publish this work. The authors are grateful to
is delayed (Figs. 13 and 14). Defense Research and Development Establishment, Gwalior,
The oscillator configuration may have indirect contribu- India, for support in various ways.
tion to the signal generation through setting the phase point
of oscillation and the pullability. If the slope of the phase
response is smaller, then more chemically sensitive oscilla- References
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[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.

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