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Microsyst Technol (2007) 13: 563567

DOI 10.1007/s00542-006-0216-x

T E C H N I C A L P A PE R

Yeolho Lee Geunbae Lim Wonkyu Moon

A piezoelectric micro-cantilever bio-sensor using


the mass-micro-balancing technique with self-excitation

Received: 31 August 2005 / Accepted: 20 January 2006 / Published online: 10 June 2006
 Springer-Verlag 2006

Abstract A biosensor was developed for using in a LabOn-a-Chip (LOC). The sensor detects the change in the
resonance frequency of a micro-cantilever with a piezoelectric lm. This is the mass micro-balancing technique, which has been successfully used for detecting
bio-materials in the quartz crystal microbalance (QCM).
The PZT lm, a piezoelectric lm, is designed to act as
both sensor and actuator. The geometry of the micro
cantilever is optimized to maximize the sensitivity and
minimize the environmental eects such as viscous
damping and added mass eect in liquid. The fabricated
sensor is composed of a 100 lm long, 30 lm wide, and
5 lm thick cantilever with a 2.5 lm thick piezoelectric
(PZT) layer on it. The ratio of thickness to length of the
micro cantilever is very high compared to others in micro cantilever-based studies. This high aspect ratio is the
key to maximize the sensitivity and minimize the environmental eects. The fabricated micro sensor was tested by detecting the mussel gluing protein, the insulinanti insulin binding protein and the poly T-sequence
DNA.

1 Introduction
Recently various sensors using a micro cantilever such as
biochemical sensors, mass sensors and biosensors have
been vigorously studied. These studies are focused on
detecting specic biomaterials or measuring biological
properties (Su Ming et al. 2003; Battiston et al. 2001; Ilic
et al. 2000; Kim et al. 2000; Baselt David et al. 1996,
Y. Lee (&) G. Lim W. Moon
Department of Mechanical Engineering,
Pohang University of Science and Technology,
San 31 Hyoja-dong Nam-gu, Pohang,
Kyungbuk 790-784, Korea
E-mail: yeolho@postech.ac.kr
Tel.: +82-54-2798217
Fax: +82-54-2795899

1997). Most of them adopt the mass micro balancing


technique which can detect very small amount of
material by measuring the change of a vibration frequency due to the mass of the material.
In the previous studies on detection of biomaterials
(Su Ming et al. 2003; Battiston et al. 2001; Ilic et al.
2000; Kim et al. 2000; Baselt David et al. 1996, 1997),
the resonance frequency of a micro cantilever was
measured by a bulky optical detection system using a
laser and position sensitive detector (PSD). However the
optical detection is not appropriate for a LOC because
much external equipment is needed. Also, the environmental conditions considered in those researches are just
in air or in vacuum, which are not realistic for a sensor
in a LOC. In addition, the sensitivity of the conventional
detection method may change drastically if the damping
increases due to the viscous eects in liquids, since it is
dependent on the change in the phase lags or amplitudes
of cantilever vibrations. This is because conventional
micro cantilevers for an atomic force microscope (AFM)
are used in the previous studies.
Therefore, in this article, a micro cantilever biosensor
actuated by a piezoelectric PZT lm is developed to
overcome these limitations for application to a LOC.
The micro biosensor is self-oscillated at its fundamental
vibrant frequency by an oscillating circuit and the
vibration frequency is measured by a frequency counter.
Since the oscillating circuit and the frequency counter
can be made small and external equipment such as a
laser and a PSD is not needed, the developed biosensor
can be applied to a LOC. Also, environmental conditions like viscous damping and added mass eect in liquid are considered in the design process. From the
structural analysis in the design process, the cantilever
becomes thick and hence it has higher aspect ratio than
other micro cantilever-based sensors. This high aspect
ratio of the micro cantilever can maximize the sensitivity
and minimize the environmental eects.
The developed biosensor is composed of a micro
cantilever and a PZT lm. The length, the width and the
thickness of the micro cantilever are 100, 30 and 5 lm,

564

respectively, and the PZT lm is 50 lm in length and


2.5 lm in thickness. The micro biosensor is tested by
detecting the mussel gluing protein, the insulin-anti
insulin binding protein and the poly T-sequence DNA.

2 Sensitivity
2.1 Dening and deriving the sensitivity
The sensitivity is dened as the ratio of the change of the
rst resonant frequency to the mass of the attached
biomaterial as equation (1).
Df
Dm

The rst resonant frequencies f0, before attaching the


biomaterial, and f, after attaching the biomaterial are
(Pilkey Walter 1994)
r
r
1
k
1
k
; f
2
f0
2p 0:07m
2p Dm 0:07m
Where k, m and Dm are stiness of the micro cantilever,
mass of the micro cantilever and mass of the attached
biomaterial respectively. Thus, the frequency shift Df is
)
r(
1
k
1
Df f0  f
1  p
3
2p 0:07m
1 Dm=0:07m
In Eq. (3) since Dm/m << 1, Taylors expansion can be
applied, and at the same time the stiness k, as expressed
by the geometry and physical properties of the micro
cantilever such as length (L), width (b), thickness (t),
elastic modulus (E) and density (q) (Pilkey Walter 1994),
is substituted to the Taylors expansion equation of Df.
Then the sensitivity becomes
  1=2  
Df
1
E
1
 30
4
3=2
Dm
2p
bL3
q

2.2 Eect of the geometry on the sensitivity


The relationship between the sensitivity and the ratio of
the resonant frequency to the mass of the micro cantilever is (Ferrari et al. 1996)
   
 Df  fn 
 / 
5
Dm  m 
and the above relationship in liquid is expressed as (Rao
Singiresu 1995)
   p2
  

 Df  
f
d
 1 fn 1  f
 /

Dm m m
M
2p
liquid
 r


1
c2 k 1=2
1
6

2p
4Mk M 3=2

Where fd , fn , mliquid , f, c and M are the damped and the


undamped resonant frequencies, the added mass of
liquid, the damping ratio, the damping coecient and
sum of the mass of the micro cantilever and added
liquid, respectively. From Eq. (5) and (6) the sensitivity
increases as the vibrant frequency increases. The value of
mliquid is expressed by multiplying the density of the
liquid and volume of the micro cantilever (q0V) (Blevins
Robert 1990), therefore mliquid is a xed value. In Eq.
(6), since the values of c and M are xed, if the stiness is
increased then the term c2/4Mk is decreased. Thus the
sensitivity is increased and the viscous damping eect (c)
can be overcome when the stiness is increased. Also,
since the stiness is proportional to t3 (Pilkey Walter
1994), therefore a thick micro cantilever can maximize
the sensitivity and minimize the environmental eects.
The length (L) and the thickness (t) of the micro
cantilever are 100 lm and 5 lm, hence it is very thick
and has a high aspect ratio, t/L = 1/20, compared to
other cantilever sensors (Battiston et al. 2001; Ilic et al.
2000; Baselt David et al. 1996; Lavrik Nickolay and
Datskos Panos 2003; Maute et al. 1999). The value of
the aspect ratio being 1/20 is not absolute standard, but
considering the value less than 1/100 in various cantilever sensors and scanning probe microscopy (SPM)
(Miyahara et al. 2002; Lee Chengkuo et al. 1999) it is
thought that this micro cantilever is sti enough to
overcome the environmental eects and consequently
have high sensitivity in liquid.

3 Fabrication and characteristics of the PZT-micro


cantilever
The fabrication processes of the PZT- micro cantilever is
depicted in Fig. 1. (1) By thermal oxidation, SiO2 was
deposited on a SOI wafer as an electrical insulation layer
between the bottom electrode and the silicon of the SOI
wafer. The bottom electrode layer, Pt/Ti, was deposited
by sputtering and a 2.5 lm thick PZT layer was coated
by the sol-gel method. And a top electrode layer, Pt, was
deposited by sputtering on the PZT. (2) The top and the
bottom electrodes were made by dry-etching using the
Ar and Cl2 reaction gas, and the PZT was dry-etched by
the Ar, Cl2 and CF4 reaction gas. (3) To insulate the top
and bottom electrode, a 5000 A thick SiO2 layer was
deposited by ion assisted deposition (IAD) and dryetched. Next, (4) an Au/Cr contact pad was constructed
by lift-o in order to connect the top electrode. (5) The
initially deposited SiO2 layer by thermal oxidation was
removed and the shape of the cantilever was formed by
ICP-RIE. (6) The thermally oxidized SiO2 on the
backside of the wafer was removed, and the backside of
the wafer was dry-etched by ICP-RIE to release the
micro cantilever. (7) The SiO2 layer of the SOI wafer
was removed by buered oxide etchant (BOE). Figure 2
shows the fabricated PZT-micro cantilever.
Various electromechanical characteristics of the fabricated PZT-micro cantilever were measured. Figure 3 is

565
Fig. 1 Fabrication process of
the PZT-micro cantilever

(1) Pt/PZT/Pt/Ti/SiO2 Deposition

(5) SiO2 and Si (cantilever) Etching

(2) Pt/PZT/Pt/Ti Etching

(6) Removing Back side SiO2 and


Back side Si Etching

(3) Isolator(SiO2) Deposition and Etching

(7) Removing Buried SiO2

Si

Pt

Pt/Ti

PZT

SiO2 Au/Cr

(4) Forming Contact Pad

the impedance around the rst resonant frequency. In


Fig. 3 the fundamental resonant frequency was about
1.3 MHz and it was close to the result of numerical
simulation which was 1.21 MHz by FEM analysis using
the ABAQUS. Figure 4a shows the vibration response
of the micro cantilever in air when a rectangular impulse
was inputted, and the micro cantilever vibrated at its
fundamental mode. Figure 4b is rectangular pulse input
test in liquid (puried water). The rst resonant frequency was about 1.1 MHz and it was decreased about
0.2 MHz. And, it was thought that this decrease of the
resonance frequency occurred due to added mass of liquid. The time duration of free vibration and the
mechanical deection were decreased about 10% and

Fig. 2 SEM image of the PZT-micro cantilever

2550% by the viscous damping of the liquid. However,


since the rst resonant frequency in liquid was still very
high, the sensitivity should not be seriously decreased
according to equation (5) and (6). Therefore, it is
thought that the micro cantilever sensor may work well
in liquid if proper surface treatment is electrically isolated the electrode.

4 Detecting biomaterials
The developed biosensor measures the change of the
vibration frequency of the micro cantilever to detect a
biomaterial because the sensor adopts the mass micro

Fig. 3 Impedance of the PZT-micro cantilever

566

Fig. 5 Self-oscillation of the PZT-micro cantilever

vibrant frequency change due to the mass of the attached biomaterials was measured by the frequency
counter. The amount of change of the resonant frequency due to the mussel gluing protein, the insulin-anti
insulin binding protein and the poly T-sequence DNA
were 85, 217 and 17.7 kHz, respectively. And the masses
of the biomaterials were estimated to be 0.1798 1015,
0.45821 1015 and 37.375 1015 g for the mussel
gluing protein, the insulin-anti insulin binding protein
and the poly T-sequence DNA respectively by substituting the measured frequency change Df, the elastic
modulus of the micro cantilever E, E = 112 GPa, and

Fig. 4 Vibration response to rectangular pulse input

balancing technique. The micro cantilever with the PZT


lm is self-excited by an oscillating circuit. The oscillating circuit can generate an oscillation signal, whose
frequency is the same to the resonant frequency of the
PZT-micro cantilever, and it feeds back the oscillatory
signal to the PZT lm. Therefore the sensor can vibrate
continuously at its rst resonant frequency. In Fig. 5,
the upper signal is the self-excitation signal of the micro
cantilever and the lower one is the feedback signal.
The micro biosensor was tested by detecting the
mussel gluing protein, the insulin-anti insulin binding
protein and the poly T-sequence DNA(5-Thiol (C6)TTT TTT TTT TTT TTT TTT TTT TTT TTT TTT-3).
The detection was processed in three steps. First, the
fundamental vibrant frequency was measured by a frequency counter. And the second step was the attachment
of the biomaterials on the gold probe area of the end of
the micro cantilever as shown in Fig. 6. Lastly, the rst

Fig. 6 Attaching the biomaterial to the PZT-micro cantilever

567

the density of the micro cantilever q, q = 2330 kg/m3,


into the sensitivity equation (Eq. 4).
The upper bound amount of mass of the biomaterials
attached on the gold area at the end of the micro cantilever was calculated under the assumption that there
are all the molecules that are possible to be attached on
the gold area. The comparison between the calculated
and the measured masses will provide with assurance
that the measured values are realistic. The calculated
maximum mass of the mussel gluing protein, the insulinanti insulin binding protein and the poly T-sequence
DNA (5-Thiol (C6)-TTT TTT TTT TTT TTT TTT
TTT TTT TTT TTT-3) were 6.393 1013 g,
0.595 1015 g and 80.167 1015 g, respectively. By
comparing the measured values with the calculated ones,
it can be seen that the measured ones are considerably
less than the calculated ones, hence, it may be concluded
that the results of the detection experiments were
meaningful.

5 Conclusion
The relationship between the geometry of the micro
cantilever and sensitivity was studied. From the relations, the dimensions of the micro cantilever, which had
a high aspect ratio, and the PZT lm were determined
and fabricated. The length, the width and the thickness
of the micro cantilever were 100, 30 lm and 5 lm, and
the dimensions of the PZT were 50 lm in length and
2.5 lm in thickness. The rst resonant frequencies of the
PZT-micro cantilever were about 1.21.3 MHz in air
and 1.1 MHz in liquid. The oscillating circuit was
composed, and the micro cantilever was self-oscillated at
its fundamental mode by the oscillating circuit. Finally,
using the self-excited micro cantilever several biomaterials were detected, and their mass were estimated. The
measured mass values using the developed cantilever
sensor were realistic when they are compared with the
theoretically-calculated upper bound of attached mass.
From the detection of some biomaterials the performance of the micro cantilever was veried, and the micro cantilever sensor can be applied to a LOC.
Acknowledgements This work is supported partly by the Next
Generation New Technology Development project (Project Number: 00013107), and partly by the Development of Next-Generation

New Technology project (Development of Intelligent Robot


Technologies for Laboratory Medicine by Applying Biotechnology, Project Number: 10024719) from the Ministry of Commerce,
Industry and Energy of Korea.

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