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Article history: The main objective of this article is to demonstrate by performing experimental measurements how the
Received 1 September 2015 equivalent capacitance C0 changes when a fluid sample such as water is in contact with the crystal and to
Received in revised form 7 December 2015 relate this change with the relative permittivity of the fluid. These measurements were compared with
Accepted 11 January 2016
simulations of traditional models like Butterworth–Van Dyke (BVD). To obtain the change of C0 when the
Available online 14 January 2016
crystal is in contact with water, the relation between the series resonance frequency (fs ) and frequency
at minimum impedance with zero phase (fr ) is used. To know these values, a new way of finding principal
Keywords:
parameters in quartz crystal resonator (QCR) sensors, such as series resonant frequency (fs ), half band
QCR
Susceptance half width ( ) and maximum peak of conductance (Gm ), is proposed; both for an unperturbed crystal and
Conductance a crystal loaded with a liquid. The method consists in measuring the current (I) that flows through the
Resonance frequency crystal and the voltage (V) between electrodes at frequency values near to resonance (sweep frequency).
Impedance analysis Additionally, the susceptance |B| of the crystal is also measured, multiplying the 90 degrees shifted current
of the crystal and its voltage, using a mixer. The DC component of this operation is proportional to the
susceptance of the crystal. With the magnitudes of the admittance and susceptance, the real value of the
conductance |G| is obtained for each frequency value in the sweep. The conductance and susceptance
curves were fitted with a summation of Gaussian and sine functions respectively with the minor RMSE
possible.
The proposed method has been compared with simulations done in COMSOL Multiphysics in order to
verify the experimental results with simulation data. MATLAB curve fitting toolbox was used to fit the
experimental curves.
© 2016 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
http://dx.doi.org/10.1016/j.sna.2016.01.021
0924-4247/© 2016 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.
0/).
154 L.A. Carvajal Ahumada et al. / Sensors and Actuators A 239 (2016) 153–160
Fig. 3. Circuit schematic sensor system containing an oscillator (10 MHz), a mixer chip (AD835), a toroidal transformer used as current sensor and conditioning stage for
signals.
value of the conductance matches with the zero susceptance value and secondary coils (1:1). The voltage signal (V2 ) related with the
independently of the properties of the sample. In other words, at current through the crystal (I1 ) and the voltage used to stimulate
resonance, the behavior of quartz crystal is purely resistive. Even, the crystal (V1 ), are multiplied in a second mixer AD835 according
C0 is considered negligible so is compensated externally with other to Fig. 3. The signal resulting is filtered using an active filter with
capacitor and according with Eq. (11) its value only depends of LT1057 Amplifier to obtain the DC component. The DC component
quartz crystal parameters. is related with the susceptance of quartz crystal according with the
However, in the obtained experimental results, the zero- following equations:
crossing point of the susceptance curve and the maximum peak
of the conductance mismatch when the crystal is in contact with V1 = Vp cos ω1 t + 1 (12)
liquid. This phenomenon occurs because C0 value also depends on
I1 = Ip cos ω2 t + 2 (13)
the properties of the sample. In other words, in the electrical model
BVD, the C0 parameter is not negligible and may even provide addi-
k
frequency (fs ) value, the frequency at minimum impedance with V1 V2 = Vp Ip cos (ω1 + ω2 ) t + 1 + 2 + ⁄2
2
zero phase (fr ) value, the half band half width ( ) value, maximum
peak of conductance (Gm ) related to the value of the motional resis- +cos (ω1 − ω2 ) t + 1 − 2 − ⁄2
tance (Rq = 1/Gmax ) and the C0 value related with sample dielectric
properties.
As ω1 = ω2 because the signal of voltage on the crystal and the
signal of current through the crystal have the same frequency, the
2.1. Stage 1—acquisition data Eq. (15) can be rewritten as:
The proposed circuit obtains the voltage and current values for k
V1 V2 = Vp Ip cos 2ω1 t + 1 + 2 + ⁄2 + cos 1 − 2 − ⁄2 (16)
several frequencies in a configurable bandwidth near to the crystal 2
resonance frequency (fc ). This circuit is a variation of Nakamoto and Then, by using a low pass filter, the high frequency component
Kobayashi proposal [14]. is removed:
The circuit consists of an oscillator chip that generates a square
k
signal of 10 MHz of frequency; its signal is filtered with a pas- V1 V2 = Vp Ip cos 1 − 2 − ⁄2 (17)
sive band-pass filter to obtain the fundamental frequency of the 2
signal. The filtered signal (sinusoidal wave) is multiplied with a The following trigonometric identity is used to get the final
sinusoidal DAQ signal using a mixer (AD835AN – Analog Devices). equation:
The resulting signal is filtered and used to stimulate the quartz crys-
tal. The frequency of the resulting signal is controlled changing the Sin (A) = Cos A − ⁄2 (18)
frequency of DAQ signal.
k
The quartz crystal is placed in series with a toroidal-core trans- V1 V2 = Vp Ip sin 1 − 2 (19)
2
former used as current sensor. The current is detected using the
toroidal transformer. The secondary coil of the transformer gives Since the relation in the toroidal transformer is 1:1, the constant
a voltage proportional to the current in the primary which is the k ≈ 1 so:
crystal current. The voltage is shifted 90 degrees with respect to the vp vp
Mixer output (DC component)= sin 1 − 2 ≈ |B| (20)
original current signal. The number of turns is the same for primary 2
156 L.A. Carvajal Ahumada et al. / Sensors and Actuators A 239 (2016) 153–160
Fig. 5. Curves for bare crystal. Magnitude of conductance |G| (green), magnitude of
susceptance |B| (blue), admittance phase curve (red).
|G| = |Y|2 − |B|2 (21)
Fig. 7. Mesh of crystal geometry in COMSOL multiphysics. The enlarged image corresponds to the mesh in thickness axis.
Table 1 Table 3
Measures for unperturbed crystal. Measures for crystal in contact with water.
Experiment Rq (ohm) Fs (Hz) Rho (Hz) Experiment Rq (ohm) Fs (Hz) Rho (Hz) Cw (pF)
Table 2
Results for bare crystal. BVD model 2 has the same BVD model parameters to except Rq correction.
BARE crystal
Table 4
Results for crystal in contact with water. BVD model 2 has the same BVD model parameters to except Rq and C0 * corrections.
Water sample
Table 5
Comparative between simulation models and experimental results for F and .
3D model BVD model BVD model 2 Experimental results %Error 3D model %Error BVD model %Error BVD model2
Rq + RL = 202.2 ± 1.9 and the value of the half band half width Rho- Through the Kanazawa Eq. (3), the viscosity of water obtained is
= 2904.8 ± 97.1 Hz. The capacitance obtained due to the water L = 9.98E–4 Pa s. The official value of the water viscosity is 1E3 Pa s
sample is Cw = 7.9 ± 0.8 pF. measured with the viscometer Fungilab (alpha series). Is impor-
The capacitance obtained due to the water sample (Cw ) is tant to highlight that the quantity of fluid used to calculate the
very similar to the value got by Rodahl et al. in 1996 [23]. viscosity using the viscometer was 20 mL, while the quantity of
The value obtained by Rodahl was Cw = 7.7pF for non-conductive fluid deposited on the QCR was only 20 l. The relative error in the
water. measure was: 0.2%.
Using the equation proposed by Rodahl et al. (Cw = 0.095
r pF),
the relative dielectric constant for the water sample obtained is
r = 83.47. This value is very close to the official value for Milli-Q 4. Conclusions
water which is 81.
Table 4 shows the data of the 3D model and BVD model simu- The model BVD is appropriated to obtain values to viscosity in
lation comparing them with the experimental results. In this case, samples with known density. However, if one considers that the C0
like for the Unperturbed Crystal, a “BVD model 2” is calculated by value also depends on the fluid sample, it is possible with the QCR
changing the value of the theoretical Motional Resistance by the used in liquids, to know additional properties of samples, differ-
value of the Motional Resistance obtained experimentally. Addi- ent to viscosity or density, characterizing not only the conductance
tionally, the C0 value is replaced too by C0 *, which is obtained from curve but also the susceptance and phase curves of the crystal.
the measures. The relation between the series resonance frequency and the
All variables of interest are very similar and save coherence with frequency at minimum impedance with zero phase when the crys-
the expectative. The multiphysics simulation generates better Q- tal is in contact with a fluid sample is directly related with the
factor because it does not contain external losses, BVD model 2 change in capacitance C0 . The change in the capacitance C0 is asso-
with Rq and C0 * corrections are closer to the experimental results. ciated with the dielectric properties of sample.
To calculate F and the procedure described in the theory The proposed system allows knowing the variables of inter-
section is used. est to characterize the unperturbed crystal and the crystal loaded
The results presented in Table 5, are obtained by subtracting the with liquids. It also allows relating quantitatively the mismatch
series resonance frequencies (fs ) and the half band half width ( ) between series resonance frequency and zero phase frequency with
for the unperturbed crystal and for the crystal in contact with a the dielectric effect of the non-conductive water. Additionally, the
liquid, for the simulation model and experimental results respec- required quantities of the sample for the proposed system are in
tively. order of microliters, while the traditional methods need milliliters
F = Fcontactwithliquid − Funperturbedcrystal of fluid to calculate the viscosity (viscometer).
= contactwithliquid − unperturbedcrystal In future works, it is expected to improve the sensor design to
The results of the 3D model differ from the other results because characterize viscosity and dielectric properties in different biolog-
the model does not consider any external loss, for example: the ical fluids. Additionally, it is aimed to perform tests with biological
external electrical circuit or the crystal manufacturing or its assem- cellcultures to obtain results of interest in the determination of
bly in the sensing system. mechanical and electrical properties of cells during its growth.
The models BVD, BVD 2 and the experimental results are very
close in F. This is consistent because the adjustments made in BVD
model 2 do not affect the value of the resonant frequency and, in Acknowledgements
general, the BVD model gives a good representation of the behavior
of the crystal. The half band half width value in BVD model 2 is a The authors thank Research and Technological Development
little closer to experimental result than the value in the BVD model. Centre of electrical, electronical and ICT industry (CIDEI) for its par-
However the difference is less significant than for the values shown ticipation with ideas and developing of prototype system. We also
in Tables 2 and 4. thank participants of Bioinstrumentation and Nanomedicine group
Finally, the value of the viscosity of the water was obtained in Center for Biomedical Technology (CTB) for its recommenda-
with the aim of validating the procedure described above and tions and loan of equipment. We thank COLCIENCIAS for supporting
the values obtained in Tables 2, 4 and 5. The utilized values this work through the grant No. 0375 – 2013 with number project
were: n = 1, f0 = 9985755.9 Hz, L = 1000 kg/m3 , L = 2651 kg/m3 , 6570577636375 and Universidad Central (Colombia) for support-
Gq = 2.93 × 1010 N/m2 , F = 2017 Hz. ing this work through the Research Cluster on Converging Sciences
and Technologies (NBIC).
160 L.A. Carvajal Ahumada et al. / Sensors and Actuators A 239 (2016) 153–160
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