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A MEMS Capacitive pH Sensor for High Acidic and

Basic Solutions
Md. Shamsul Arefin*, M. Bulut Coskun+, Tuncay Alan+, Adrian Neild+, Jean-Michel Redoute, Mehmet R. Yuce *
*

Department of Electrical and Computer Systems Engineering, Monash University, Melbourne, VIC/Australia,
+
Department of Mechanical and Aerospace Engineering , Monash University, Melbourne, VIC/Australia
Email: {md.arefin, bulut.coskun, tuncay.alan, adrian.neild, jean-michel.redoute, mehmet.yuce}@monash.edu

Abstract We have developed a micro-scale chip-based pH


sensing system, which can effectively measure the changes in pH
ranging from 1 to 4 and 10 to 12. This method relies on fringing
field capacitive measurements. A change in pH of the medium
results in a permittivity change for the fringing electric field,
which in turn affects the capacitance values. Capacitance
changes are then converted to resonant frequency shifts via a
readout circuit. This technique provides high sensitivity, low
hysteresis, and low noise as well as low fabrication cost. Very
importantly, the device and the corresponding measurement
circuitry have the potential to be integrated in an electronic pill
for continuous non-invasive measurement within the body.
KeywordspH sensor; MEMS; capacitive; fringing field

I.

INTRODUCTION

Conventional methods to measure pH such as


potentiometric [1] and glass electrode [2], rely on Nernstian
response of reactions at a solid-liquid interface. Although the
glass electrode method is the standard measuring method for
pH due to ideal nernstian response independent of redox
interferences, it shows sluggish response, causes inconsistent
results in HF or alkaline solutions, requires conducting sensing
materials, and especially presents unstable response for
miniaturized systems [2].
Moreover, other sophisticated methods are emerged to
overcome the limitations of potentiometric and glass
electrodes as well as to operate the sensor in various chemical
and biological environments. First, the conductometric method
utilizes the conductivity of a pH-responsive conducting
polymers [3]. Second, magneto-elastic method senses the
vibrations induced by magnetic fields on the magneto-elastic
ribbons coated with pH responsive hydrogel [4]. The polymer
layers and device fabrication processes for this methods could
be expensive and complicated [2]. Third, optical fiber method
is based on evanescent-wave spectroscopy employing the
color changes of sensing polymers having pH solutions with
negligible ionic concentrations [5]. This method includes
optical devices that might be unsuitable for miniaturized
systems. Fourth, microcantilever-based method utilizes the
surface stress induced bending of microcantilever coated with
pH-sensitive polymers [6]. However, fabrication process of
polymer based microcantilever might be difficult due to creep
deformation and ageing. Moreover, the instability of the
sensor during measurements might also pose a problem [6].
Lastly, ISFET measures the current through a conduction

978-1-4799-0162-3/14/$31.00 2014 IEEE

channel between source and drain originating from pH


dependent threshold voltage due to sensing gate-liquid surface
potential [7]. This technique requires higher power for FET
operations, sophisticated fabrication process due to
encapsulation of drain, source, and chip edges area except gate
area, prone to electrostatic damage of gate oxide, and is
difficult to integrate into a miniaturized system due to floating
gate configurations [8].
Despite having the capability to measure a wide range of
pH, these methods are either difficult to integrate into
miniaturized systems or exhibit unstable or weak responses for
strong acidic or basic region.
Here, we present a miniaturized chip based (350 m x 270
m) capacitive pH sensor [9] and corresponding interface
circuit to overcome limitations of conventional techniques for
continuous real-time measurements of high acidic and basic
medium. The device can effectively measure pH levels from 1
to 4 and pH levels from 10 to 12. It also has the potential to
measure gastric acid (typical pH levels 1-2 [10]) and to
integrate the techniques into miniaturized electronic pill
systems [11]. This method offers high sensitivity, reliability
and repeatability for strong acidic and basic pH levels as well
as reduces the fabrication complexity and cost.

Fig. 1. Design of the fringing field capacitive pH sensor. There are 5 pairs
of gold electrodes (L: 200m, W:10m, Spacing:10m) in the sensing
area. As shown in the cross-sectional view, sensor is composed of 4
layers, namely; 500m-thick Si, 500nm SiO2, 300nm Au and 5nm
Si3N4.

II.

SENSOR DESIGN AND PRINCIPLE

We have developed the device shown in Fig. 1 using


conventional microfabrication steps. Briefly, a set of IDEs and
conducting pads were patterned on a silicon (<1 0 0> oriented)
Si substrate covered with a 500nm-thick silicon dioxide (SiO2)
layer. The top surfaces of IDEs were passivated by silicon
nitride (Si3N4) layer to provide sensing surface for pH buffer
solutions as well as to limit Faradiac currents between the
electrodes. The IDEs, having each electrode width of 25m
and length of 200m, and inter-electrode spacing of 10m,
were fabricated.
The principle of operation of the sensor is based on the
logarithmic relation between the number of H+ or OH- ions in
a solution (and correspondingly the permittivity) and pH.
When a solution is placed on top of the sensing electrodes
(Fig. 1), H+ modifies the fringe electric fields generated by the
electrodes. That leads to a change in permittivity, which in
return alters the capacitance value.
An electric double-layer of H+-ions forms at the nitridesolution interface due to the electric fields. The surface
charges at nitride layer act as a source or sink of the H+-ions
in the solutions. An electric double-layer capacitance forms at
the interface that depends on the concentration of H+-ions of
the solutions.
In the solution bulk, a diffuse-layer capacitance is formed
due to the free H+-ions in the solutions. Local electric fields
around the ions interact and attenuate with the external electric
fields in the solution bulk. The attenuation is higher for higher
concentration of H+ and OH- ions. Hence, lower pH decreases
the dielectric constant. The change of frequency-dependent
dielectric constant for different pH solutions is reflected as the
change in capacitance of the sensor.
III.

INTERFACE CIRCUIT

The capacitive changes due to pH changes are converted to


frequency variations using a frequency-modulation based
interface circuit, as shown in Fig. 2. The interface circuit is
implemented using a differential crossed-coupled voltage
controlled oscillator (VCO). The sensor (Csen) is connected
parallel to an inversion-MOS (I-MOS) varactor (C0) and
inductor (L0) acting as an LC-tank of the VCO. The VCO
oscillation frequency can be approximated as;

f vco

1
2 L0 (C0 C sen )

Fig. 2. Schematic of the voltage controlled oscillator (VCO)


that converts the changes in capacitance to resonant frequency
shifts.

is high within the test range. Hence, instead of detecting


capacitive changes in the order of pF range, the output of the
sensor can be observed by means of highly detectable resonant
frequency shifts.
IV.

EXPERIMENTAL PROCEDURE AND RESULTS

In order to characterize the sensor, commercially available


standard buffer solutions were used. For each solution, pH
values were first measured by a commercial glass-electrode
pH meter (HI98128, HANNAInstruments) prior to the
experiments.

(1)

The advantage of the oscillator readout circuit comes from


the inversely proportional nonlinear relation between the
resonant frequency and sensor capacitance, as shown in (1).
Note that, this type of relation exhibits the best performance
when initial sensor capacitance is small and percentage change

Fig. 3. An image of the fabricated chip wire-bonded to the pin grid array
that is placed on the VCO.

ACKNOWLEDGMENT
Part of this work was performed at the Melbourne Centre
for Nanofabrication (MCN) in the Victorian Node of the
Australian National Fabrication Facility (ANFF).

REFERENCES
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Fig. 4. The resonance frequency of VCO for strong acidic buffer


solutions (pH 1 to 4) and for strong basic buffer solutions (pH 10 to 12)
in the inset.

After sensor is placed on top of the interface chip (Fig. 3), a


drop of pH solution was placed on top of the electrodes and
corresponding oscillation frequency of VCO circuit was
measured using a spectrum analyzer (Rohde&Schwarz FSH3).
By repeating the procedure with different pH buffer solutions,
we mapped the frequency output of the VCO to corresponding
pH values for pH 1.0 to 4.0 and acquired a total frequency
change of 30.55 MHz (Fig. 4). Since the molar concentrations
of H+ ions are higher in strong acidic region, the sensitivity is
very high at low pH levels. Similarly, OH- concentrations are
higher for a strong basic region that leads to a larger change as
the pH increases, as shown in Fig. 3 inset. Total frequency
shift within pH10-12 range is 4.317 MHz.
V.

CONCLUSION

This work presents a capacitive technique to measure the


strong acidic and strong basic ranges utilizing the fringe
electric fields. The changes in sensor capacitance,
corresponding to pH levels are measured using frequency
modulation technique. This method offers high resolution, low
noise in measurements as well as a low cost fabrication
process.
Future work will focus on wireless sensor data
transmission as well as shrinking the form factor of the chip
and the readout circuit further down to fit the whole system
into an electronic pill.

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