IEEE TRANSACTIONS ON NANOTECHNOLOGY, VOL. 11, NO.

4, JULY 2012

701

Piezoresistive SU-8 Cantilever With Fe(III)Porphyrin

Coating for CO Sensing
C. Vijaya Bhaskar Reddy, Mrunal A. Khaderbad, Sahir Gandhi, Manoj Kandpal, Sheetal Patil, K. Narasaiah Chetty,
K. Govinda Rajulu, P. C. K. Chary, M. Ravikanth, and V. Ramgopal Rao, Senior Member, IEEE

AbstractCarbon monoxide detection is required for various healthcare, environmental, and engineering applications.
In this paper, 5,10,15,20-tetra (4,5-dimethoxyphenyl)-21H,23Hporphyrin iron(III) chloride (Fe(III)porphyrin) coated on a
piezoresistive SU-8 microcantilever has been used as a CO sensor.
Rapid detection of CO down to 2 ppm has been observed with aforementioned sensors. Cantilevers without Fe(III)porphyrin have not
responded to CO exposure. Fe(III)porphyrin-coated cantilever selectivity toward CO has been analyzed by measuring the sensor
response to various gases such as N2 , CO2 , O2 , ethanolamine,
N2O, and moisture. The sensor has exhibited a fast response and
recovery times and is fully recoverable after repeated exposures.
Index TermsCantilevers, carbon monoxide, iron porphyrin,
piezoresistance, sensor.

I. INTRODUCTION
ONSIDERING its omnipresence, carbon monoxide (CO)
is one of the most harmful compounds for human beings.
CO can jeopardize oxygen transport in blood and it is one of the
most important gases to be detected for gas sensor-based fire
detection [1] applications. The efficiency of fuel combustion in
combustion engines, power plants, fuel cells, and automobiles
can be monitored by quantifying CO emission. This provides
information not only for feedback control of combustion processes, but also to indicate various fire and health hazards [2].
This demand has stimulated research to realize low-power sen-

Manuscript received January 6, 2012; accepted February 24, 2012. Date

of publication March 12, 2012; date of current version July 11, 2012. This
project is supported by the Department of Information Technology, Ministry
of Communication and Information Technology, Government of India under
the Indian Nanoelectronics Users Program (INUP) at Indian Institute of
Technology Bombay (IIT Bombay). The review of this paper was arranged by
Associate Editor J. Li.
C. V. B. Reddy is with the Department of Mechanical Engineering, Srikalahasteeswara Institute of Technology, Srikalahasthi 517640, India (e-mail:
bhaskarreddychalla@gmail.com).
M. A. Khaderbad, S. Gandhi, M. Kandpal, and V. Ramgopal Rao are with the
Centre of Excellence in Nanoelectronics, Indian Institute of Technology
Bombay, Mumbai 400076, India (e-mail: mrunalak@gmail.com;
sahirgandhi11@gmail.com; mkandpal@ee.iitb.ac.in; rrao@ee.iitb.ac.in).
S. Patil is with the Nanosniff Technologies Pvt. Ltd., Indian Institute of
Technology Bombay, Mumbai 400076, India (e-mail: sheetal@ee.iitb.ac.in).
K. N. Chetty and K. G. Rajulu are with the Department of Mechanical
Engineering, Jawaharlal Nehru Technological University, Anantapur 515002,
India (e-mail: narasaiahchettyk@gmail.com; govindjntu@gmail.com).
P. C. K. Chary is with the Department of Mechanical Engineering,
Sree Vidyanikethan Engineering College, Tirupathi 517501, India (e-mail:
pckchary@yahoo.com).
M. Ravikanth is with the Department of Chemistry, Indian Institute of Technology Bombay, Mumbai 400076, India (e-mail: ravikanth@chem.iitb.ac.in).
Color versions of one or more of the figures in this paper are available online
at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/TNANO.2012.2190619

sors, which are compact and work in real-world conditions [3].

Various sensing elements comprising of nanomaterials to improve the selectivity and sensitivity of detection have been examined for this purpose.
The usability of copper chloride (CuCl) as a selective CO
sensor in the presence of 50 vol% hydrogen has been demonstrated for proton-exchange membrane fuel cell applications.
However, the CO sensing performance of CuCl films is very
sensitive to the synthesis and fabrication methods [4]. CO gas
sensors based on gold (Au)-doped tin oxide (SnO2 ) have shown
efficient sensing in the 80210 C temperature range [5], [6].
Pthalocyanine nickel(II)-coated piezoelectric crystal has also
been investigated as a CO sensor [7], [8]. Other types of sensors
for CO detection include electrochemical sensors, thermoelectric, colorimetric detectors, and infrared detectors [9][12].
It is well known that molecules with a central metal atom
surrounded by neutral or charged ligands have been employed
for active gas sensing, where vacant sites or weakly bound coligand interact with the metal ion. In this interaction, the gaseous
molecule to be detected becomes a co-ligand either by occupying free coordination site or by displacing other ligands. Colorimetric sensor based on the interaction between CO and porphyrin films has been explored for the estimation of the biological damage due to CO exposure [13]. Radhakrishnan et al., have
used polypyrrole functionalized with 5,10,15,20-tetraphenyl21H, 23H-porphyrin iron(III) chloride (PPyFeTPPCl) as an
active sensing material for CO gas. It was observed that semiconducting PPyFeTPPCls resistance was drastically increased
upon CO exposure [14], [15].
In this study, we demonstrate highly sensitive CO detection using 5,10,15,20-tetra(4,5-dimethoxyphenyl)-21H,23Hporphyrin iron(III) chloride (Fe(III)porphyrin)-coated SU-8
nanocomposite microcantilevers with integrated piezoresistive
readout. As compared to conventional Si-based cantilevers,
polymer (SU-8 as a structural layer)-based cantilevers provide
higher sensitivity and use low cost fabrication techniques such
as spin coating, evaporation and wet etching etc. [16], [17].
A typical (Fe(III)[T(4,5(OCH3 )2 P)P]Cl)-CO interaction modifies surface stress on the cantilever when exposed to the CO gas.
The change in surface stress results in a resistance change in the
integrated piezoresistor, thus enabling electrical detection.
II. EXPERIMENTATION
The polymer cantilevers for the fabrication of CO sensor were fabricated using the following process [17], [18].
Nanocomposite-based polymer microcantilevers of the dimensions, 200, 50, and 3.5 m, length, width, and thickness,

1536-125X/$31.00 2012 IEEE

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IEEE TRANSACTIONS ON NANOTECHNOLOGY, VOL. 11, NO. 4, JULY 2012

Fig. 1. Process sequence for polymer composite microcantilevers. (a) Silicon

dioxide as a sacrificial layer. (b) First layer of SU-8. (c) Cr/Au for contacts. (d)
SU-8/CB composite layer. (e) Encapsulating SU-8. (f) Thick SU-8 die base. (g)
Release of cantilever die from the substrate.

Fig. 2. (a) Schematic of the porphyrin molecule and SEM images of the released nanocomposite microcantilever devices. (b) Change in resistance (R/R)
as a function of deflection.

respectively, are used in this study in order to improve the

surface stress sensitivity, mechanical stability, and packaging
compatibility of the sensors. Nanocomposite, based on a dispersion of carbon black nanoparticles in SU-8, a nonconductive,
negative tone photoresist, is used as a piezoresistive layer in
these polymer cantilevers. The SU-8/carbon black nanocomposite is obtained by homogeneously mixing the carbon black
powder in the photosensitive SU-8 resin. The lower Youngs
modulus of SU-8 compared to Si and the higher strain sensitivity of SU8/carbon black nanocomposite provides these devices
the required sensitivity to detect CO down to the ppm sensitivity.
The nanocomposite polymer microcantilever fabrication process sequence is illustrated in Fig. 1. The fabrication starts with
RCA cleaning of silicon substrate with 500-nm thermally grown
silicon dioxide as a sacrificial layer. SU-8 structural layer (SU8 2000.5, Microchem, MI) was spin coated and pre-exposure
baked at 70 C and 90 C for optimized timings with a slow
ramp up and ramp down to room temperature. To transfer the
microcantilever pattern [see Layer-1, Fig. 1(b)], the samples
were exposed to UV light using Karl Suss MJB3 mask aligner
and subjected to a post exposure bake cycle, development and
rinsed with Iso Propyl Alcohol (IPA). A thin layer of Cr/Au
(10 nm/200 nm) was deposited by sputtering, and the contact
pads were patterned using PPR photolithography with the corresponding mask [see Fig. 1(c)]. The CrAu layer was wet
etched in respective enchants. To obtain an electrically conductive and a strain sensitive layer, SU-8/CB nanocomposite was
prepared by dispersing the carbon black of 89 Vol.% in SU-8.
The nanocomposite was spin coated and subsequently patterned
using mask for layer 3 [see Fig. 1(d)] by UV lithography, followed by additional ultrasonic cleaning step in IPA. This strain

sensitive resistive layer is then encapsulated by 1.6 m of SU-8

(2002) that is spin coated and photolithographically patterned
using mask for layer 4 [see Fig. 1(e)]. Finally to form an anchor [see Fig. 1(f)] for the cantilevers, a 180-m thick SU-8
was defined by spin coating and patterning of SU-8 (2100). The
devices were released by wet etching the silicon dioxide layer
in the buffered hydrofluoric acid approximately for 30 min.
The arrays of released SU-8 nanocomposite microcantilever
chips were rinsed in DI water, isopropyl alcohol and allowed to
dry. Fig. 2(a) shows the SEM images of the released microcantilever devices. The microcantilever chips were characterized
electromechanically to demonstrate the piezoresistive behavior.
The tip of the microcantilever was deflected with a calibrated
micromanipulator needle from Suss Microtech with simultaneous measurement of resistance using Keithley 4200 source
measuring unit. The change in resistance (R/R) as a function
of deflection is given in Fig. 2(b), the calculated deflection sensitivity is 1.1 ppm/nm [18], which is higher compared to the
polymer microcantilevers with Au as the strain gauge.
The piezoresistance value of the fabricated cantilevers was
measured to be 500 k. The (Fe(III)[T(4,5(OCH3 )2 P)P]Cl) was
dissolved in IPA solution (1 mg in 20 mL of solution) and the
selected cantilevers were drop coated using a microdispenser.
Further, the backside of the cantilever is coated with gold using
the Nordiko sputter machine at a base pressure of 1.0 105
mbar and sputter pressure of 2.6 103 mbar to avoid the
interaction of porphyrins with the CO vapors on the bottom side
thus enhancing the systems electrical response.
The cantilever is then mounted onto a printed circuit board
(PCB) and electrical connections were made between the cantilever and the preexisting contact leads on the PCB using

REDDY et al.: PIEZORESISTIVE SU-8 CANTILEVER WITH FE(III)PORPHYRIN COATING FOR CO SENSING

703

Fig. 3. (a) Cantilever mounted on PCB and flow cell arrangement for gas
sensing. (b) Experimental setup.

conductive silver epoxy (1:1) which included a 80 C heat treatment for curing purposes. The cantilever is then enclosed in a
flow cell made of Teflon and sealed for further measurements.
This standard flow cell has an inlet and an outlet for the gas flow
as shown in Fig. 3(a).
The experimental setup for sensor calibration used is shown
in Fig. 3(b). CO and the carrier gas (N2 ) were allowed to flow
out of the cylinders through flow controllers. The flow cell was
connected to a gas-mixing chamber as inlet and the flow cell
outlet was connected to a pump (not shown). The cantilever
sensor is connected to a Wheatstones bridge and the dc voltage
was recorded using the ADS123X TI board (Texas Instrument
Board). The wheatstone bridge consists of four arms of which
one arm is cantilever and the remaining three arms have potentiometers. Initially, the bridge is balanced by matching R4
with cantilever and R1 with R2. As the change in the resistance
R due to strain in the cantilever is very small, in orders of
few ohms in 100 k, nonlinearity error of the bridge is negligible. The output of the bridge is fed to one of the three input
channels of ADC. The strain on the piezoresistive layer of the
nanoelectromechanical cantilever results in the deflection sensitivity, which is an important performance parameter. The relative
change in the resistance (R) with respect to the fixed arm of the
bridge is determined by the deflection sensitivity. By means of
the Wheatstone bridge the change in the resistance is measured
in terms of voltage. Sensitivity calculation of the current system
is based on the change in output voltage for the corresponding
resistance change in one of the arms of the bridge.
N2 purge was carried out before the start of the experiment.
Fe(III)porphyrin-CO interaction causes the cantilever to deflect,
which changes the resistance of cantilever [14]. The change in
the resistance was measured as a voltage change in the output
[17][20].
III. RESULTS AND DISCUSSION
Fig. 4(a) shows the response of a bare SU-8/CB cantilever
for alternating cycles of CO and N2 gases at 500 sccm flow

Fig. 4. (a) Response of a bare SU-8/CB polymer composite microcantilever

for consecutive cycles of CO and N2 . (b) Response of a Fe(III)porphyrin-coated
microcantilever for consecutive cycles of CO and N2 .

rate. It can be clearly seen that the cantilevers did not respond
to either of the gasses. Similarly, the cantilevers functionalized with Fe(III)porphyrin were exposed to alternating cycles
of CO and N2 (500 SCCM) and the response is as shown in
Fig. 4(b). From the figure, it is clear that there is an abrupt
increase in the sensors response due to CO adsorption. A voltage output of 80 mV was observed on each alternating cycle,
which shows the recovery and repeatability of the sensor. The
sensor response and recovery times have been measured to be
1 and 2 s. This clearly demonstrates that only porphyrin functionalized microcantilevers respond to CO gas, while the bare
cantilevers do not respond to the CO exposure. The overall time
responses demonstrate that Fe(III)porphyrin-coated films show
a very good response to CO at room temperature and ambient
conditions.
The Fe(III)porphyrin functionalized cantilevers were then
exposed to various concentrations of CO ranging from 7 to
70 sccm and the response was plotted as shown in the Fig. 5.
The porphyrin functionalized sensor was also tested for its selectivity by exposing it to various other gases such as CO2 ,
O2 , N2 0, and ethanolamine (300 sccm). Fig. 6 shows the response indicating that the Fe(III)porphyrin functionalized cantilevers did not respond to the other gases. Output response of the
same cantilever for 300 sccm CO exposure was around 12 mV,
depicting the high selectivity of the sensor toward CO. Further, Fe(III)porphyrin and CO binding was analyzed by Fourier
transform infrared spectroscopy (FTIR). The FTIR spectra of
Fe(III)porphyrin coated on Si before and after CO exposure
is shown in Fig. 7. In the spectrum, an IR peak is observed

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IEEE TRANSACTIONS ON NANOTECHNOLOGY, VOL. 11, NO. 4, JULY 2012

firms that the Fe(III)porphyrin reported in this paper is efficient

in CO binding and the functionalized cantilevers are suitable for
CO sensing applications. Moreover, porphyrin molecules are
known to be stable in solution as well as in solid-state form,
for the long-term operation of these sensors [22], [23]. In addition, moisture effect on SU8 devices can be overcome with differential measurements and through postfabrication processes
involving hard baking. Such baking for longer times is known
to increase the polymers cross-linking density, which, in turn,
decreases the sensitivity of the material to the environmental
humidity [24], [25].
Fig. 5. Response of porphyrin functionalized SU-8/CB microcantilevers for
different CO flow rates.

IV. CONCLUSION
In conclusion, microcantilever-based CO sensor has been fabricated based on Fe(III)porphyrin-coated SU-8/CB cantilever.
Experimental results indicate that the Fe(III)porphyrin-coated
cantilevers have a very high sensitivity toward CO as compared
to bare SU-8 cantilevers. In addition, Fe(III)porphyrin-coated
cantilevers selectivity toward CO was compared by measuring
the response with gases such as N2 , CO2 , O2 , ethanolamine,
N2 O, and moisture.
ACKNOWLEDGMENT
The authors would like to thank Prof. P. Mathur, Department
of Chemistry, IIT Bombay, for CO facility.

Fig. 6. Response of porphyrin functionalized SU-8/CB microcantilevers for

different gases.

Fig. 7. FTIR spectroscopy of Fe(III)porphyrin on Si before and after CO

exposure.

around 1820 cm1 after CO exposure, which is because of the

metalCO binding frequency. This indicates that CO interacts
with the central metal ion of porphyrin, by forming a coordinate
covalent bond with Fe with its lone pair of electrons [14], [21].
Moreover, microcantilevers coated with free base tetra
phenyl porphyrin (H2 TPP) and zinc(II)tetra phenyl porphyrin
(Zn(II)TPP) were tested for CO selectivity. These cantilevers
did not show any sensing behavior toward CO. This is because
of the lack of CO binding site (no metal) in freebase porphyrin
and group 12 metals such as zinc. In Zn(II)TPP, Zn does not
bind to CO as its d-orbitals are not really available. This con-

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C. Vijaya Bhaskar Reddy received the B.E. degree

from S. V. University, Tirupathi, and the Masters degree from J.N.T.University, Hyderabad, India. He is
currently working towards the Ph.D. degree with the
J.N.T University, Anantapur, India.
He is presently working in SKIT Engineering college Srikalahasthi, India as an Assistant Professor.
His research interests are automotive sensors systems, bioinstrumentation, nanofabrication, thin and
thick film sensor systems.

705

Mrunal A. Khaderbad received the M.Tech. degree

from VNIT, Nagpur and the M.Phil. from the University of Cambridge, U.K. Currently, he is pursuing
the Ph.D. degree in Centre of Excellence in Nanoelectronics, Electrical Engineering Department, IIT
Bombay, India.
He was a Visiting Researcher at the Energy Research Institute at the NTU (Eri@N), Nanyang Technological University, Singapore. His research areas
are Cu/low-k interconnects, NEMS, Sensors, and
graphene electronics.

Sahir Gandhi is working toward the Ph.D. degree at

Imperial College London, U.K. advised by Dr. Danny
O.Hare and Prof. Martyn Boutelle at the Bioengineering department.
He is a postgraduate in biomedical engineering
from Imperial College London. He worked at IIT-B
as a Sr. Research Assistant on Lab-on-Chip devices.

Manoj Kandpal received the M.Tech degree in materials science and engineering from the Indian Institute of Technology (IIT) Kharagpur, India, in 2008.
He is currently a Ph.D. student in the Department of
Electrical Engineering, IIT Bombay, India.
His research interests includes piezoelectric
nanocomposite based devices and chemical sensors.

Sheetal Patil received the Ph.D. degree from the University of Pune, India, in
2004.
She has worked as a Research Scientist and Research Faculty, at Department
of Electrical Engineering, University of South Florida, Tampa and Bio-MEMS
Group, Department of Mechnical Engg., University of Maryland, College Park,
respectively. She has published more than 25 peer reviewed journal papers in the
fields of Microfabrication and Chem-Bio sensors. She is currently working as a
Lead Manager (R&D) in NanoSniff Tech. Pvt. Ltd., a company incubated at
IIT-Bombay, Mumbai, India.

K. Narasaiah Chetty graduated in mechanical engineering from S.V. University Tirupathi, India and
received the doctoral degree from Indian Institute of
technology Madras.
After the Ph.D. degree he joined as an Assistant
Professor at J.N.T. University, Anantapur, India. He is
a life member in Indian Society Technical Education,
Solar Energy Society of India and Indian Society of
Heat and Mass Transfer.

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IEEE TRANSACTIONS ON NANOTECHNOLOGY, VOL. 11, NO. 4, JULY 2012

K. Govinda Rajulu received the doctoral degree

from the Indian Institute of Technology, Roorkee,
India, in 1993.
After the Ph.D. degree he joined as an Assistant
Professor at J. N. T. University, Anantapur, India. He
is Fellow of Institutional of Engineers, INDIA, holds
Charted Engineer (INDIA) Certificate and Life member of Indian Society for Technical Education.

M. Ravikanth M. Ravikanth was born in Andhra

Pradesh, in 1966. He received the B.Sc. and M.Sc.
degrees from Osmania University, Hyderabad, india
and the Ph.D. degree from the Indian Institute of
Technology, Kanpur, India, in 1994.
After his postdoctoral stay in USA and Japan, he
joined as a faculty at Indian Institute of Technology,
Bombay, where he is currently a full Professor. His
current research interest includes porphyrin and related macrocycles, and boron dipyrromethenes.

P. C. K. Chary received the B.Tech, M.E., Ph.D.,

and MISTE degrees.
He is working as a Principal for Sree
Vidyanikethan Engineering College, Tirupati, India. He did his Ph.D. in CAD/CAM from Sri
Venkateswara University, Tirupati, India. He has
published 22 papers so far at National and International level. His research interests are Intelligent
CAD/CAM Systems, MEMS, FlexibleManufacturing Systems and Applications of Computers in Manufacturing.

V. Ramgopal Rao (M98SM02) is an Institute

Chair Professor in the Department of Electrical Engineering, IIT Bombay. He has over 300 publications
in the area of Electron Devices & Nanoelectronics in
refereed international journals and conference proceedings and has 16 patents issued or pending.