Pigment & Resin Technology

Effect of humidity on copper phthalocyanine films deposited at different gravity conditions

Khasan S. Karimov Zubair Ahmad Noshin Fatima Muhammad Mansoor Ahmed Muhammad Abid
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Khasan S. Karimov Zubair Ahmad Noshin Fatima Muhammad Mansoor Ahmed Muhammad Abid , (2017),"Effect of humidity on
copper phthalocyanine films deposited at different gravity conditions ", Pigment & Resin Technology, Vol. 46 Iss 1 pp. 64 - 70
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 Effect of humidity on copper phthalocyanine
films deposited at different gravity conditions
Khasan S. Karimov
Centre for Innovative Development of Science and Technologies of Academy of Sciences, Dushanbe, Tajikistan
and GIK Institute of Engineering Sciences and Technology, Topi, Pakistan
Zubair Ahmad
Department of Electrical Engineering, College of Engineering, Qatar University, Doha, Qatar
Noshin Fatima and Muhammad Mansoor Ahmed
Department of Electrical Engineering, Capital University of Science and Technology (CUST), Islamabad, Pakistan, and
Muhammad Abid
Interdisciplinary Research Center, COMSATS Institute of Information Technology, Wah Cantt, Pakistan

Abstract
Purpose The paper aims to study the effects of humidity on the electrical properties of copper phthalocyanine (CuPc) thin films deposited at
different gravity conditions.
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Design/methodology/approach Surface-type samples were fabricated on glass substrates with preliminary-deposited copper electrodes. The
CuPc solution was prepared in benzene. The thin films of CuPc were deposited on these substrates at diverse gravity conditions by drop-casting and
centrifugation at 1 g and 70 g, respectively. Impedance and capacitance of the fabricated devices were measured against the different relative
humidity ranging from 32 to 98 per cent.
Findings The impedance and the capacitance of the CuPc film were found to be dependent on the ambient humidity levels (32-98 per cent) and
the gravity conditions (1 g and 70 g) opted during the fabrication process.
Research limitations/implications The centrifugation technique can potentially be used in the instrumentation industry for the fabrication of
humidity sensors.
Practical implications The results of the investigations can potentially be used in the instrumentation and optoelectronics industry for the
fabrication of humidity sensors.
Originality/value CuPc films were deposited from a solution in benzene using drop-casting and centrifugation. The electrical properties of the
films were found to be dependent on film fabrication conditions and ambient humidity levels. Growth-dependent electrical properties of the CuPc
films can be explained by considering their structure.
Keywords Colorant, Humidity, High gravity, Centrifugation, Copper phthalocyanine, Drop-casting
Paper type Research paper

Introduction are found suitable for centrifugal processing (Regel and

Phthalocyanines are used as pigments in automotive paints,
printing inks, blue/cyan dyes for textiles and the paper
industry. Because of their versatile applications,
phthalocyanines have been the focus of interest in organic
semiconductor and photosensitive industries as well. It is an
established fact that the structures and properties of organic
semiconductors are highly dependent upon their processing
technology (Gutman and Lyons, 1981; Gutman et al., 1983).
Generally, organic materials have a high molecular weight and
strong intramolecular but weak van der Waals intermolecular
bonding. Because of these properties, organic semiconductors
Wilcow, 2000; Wilcox and Regel, 1996).
The properties of devices based on metallophthalocyanines
grown by the organic molecular beam deposition (OMBD)
technique were investigated by Colesniuc (2011). It was
reported by Colesniuc that the conductivity of the grown films
increases exponentially with temperature, whereas it decreases
exponentially with increasing the thickness of the films.
Applications of copper phthalocyanine (CuPc) include
The authors are thankful to Capital University of Science and Technology
(CUST) and Ghulam Ishaq Khan Institute of Engineering Sciences and
Technology, Pakistan, for supporting this work.

Received 23 November 2014

Revised 4 April 2015
The current issue and full text archive of this journal is available on 9 July 2015
Emerald Insight at: www.emeraldinsight.com/0369-9420.htm 23 September 2015
30 January 2016
23 February 2016
Pigment & Resin Technology 7 March 2016
46/1 (2017) 64 70 29 March 2016
Emerald Publishing Limited [ISSN 0369-9420] 17 April 2016
[DOI 10.1108/PRT-11-2014-0105] Accepted 21 May 2016

64
 Effect of humidity on copper phthalocyanine films
Khasan S. Karimov et al.
photovoltaic cells, paint, ink, etc. Organic thin-film transistors
were also fabricated using CuPc dye with the standard
vacuum evaporation method (Wu et al., 2013). These
transistors had a five-layered structure comprising of Au
(source)/CuPc/Al (gate)/CuPc/Au (drain) and exhibited a
relatively good performance. Dependence of electrical
properties of CuPc and metal-free phthalocyanine (H2Pc)
bulk heterojunction structures under varying illumination
conditions was also studied by Farooq et al. (2015). A
comparative analysis of currentvoltage (I-V) characteristics in
dark and under illumination showed that the devices were
sensitive toward visible light. Their absorption spectra exhibit
photosensitivity in the wavelength ranging from 200 to
850 nm. Touka et al. (2013) reported preparation and
characterization of CuPc nanocrystals embedded into the
polymer host and investigated optical absorption spectra of the
grown films.
A comparison of electric and optical properties of an organic
semiconductor clearly demonstrates an obvious correlation
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between the activation energy measured by the conductivity
temperature or by the absorption spectra (Brutting et al.,
2012). Similarly, the color of an organic material is dependent
on its band gap or activation energy. Encouraged from these
characteristics, the colorants films were fabricated especially in
an unconventional environment, for example at high gravity
conditions, to explore their potential use in the organic
semiconductor industry.
Previously, we reported the heterojunctions fabricated
under high gravity using p-type Si and thin films of
poly-N-epoxypropylcarbazole (PEPC) doped with
tetracyanoquinodimethane (Ahmed et al., 2004). The PEPC
films were grown on Si wafers at different gravity conditions
(i.e. 1 g, 123 g, 277 g and 1,107 g). It was observed
that the grown organic polymer films had uniform surface
morphology and good adhesiveness on Si substrate. The I-V
characteristics of the fabricated hybrid structures were
evaluated as a function of temperature ranging from 20C to
60C. It was found that all the samples were p-p isotype
heterojunctions. Rectification ratio, threshold voltage, reverse
saturation current and junction resistance of the fabricated
junctions were evaluated at different temperatures. Later on, a
theoretical model has been proposed by Hu and Chen (2015)
by developing a relationship that quantitatively linked the
centrifugal time with centrifugal conditions to fabricate
high-quality photonic crystals.
In this paper, in continuation of our efforts pertaining to
humidity and temperature sensors (Karimov et al., 2008,
2012), we are presenting humidity-dependent electrical
properties of CuPc thin films deposited at different gravity
conditions (1 g and 70 g) using the centrifugation
technique.
Experimental
Materials
For thin film deposition, commercially produced (Aldrich)
CuPc (C32H16CuN8) powder was used. Figure 1 shows the
molecular structure of CuPc. Its molecular weight is 576.08,
and it is very stable (Kumar and Ghosh, 2002). It is a
photosensitive semiconductor (Hiesgen et al., 2000) and has
65
Pigment & Resin Technology
Volume 46 Number 1 2017 64 70
Figure 1 Molecular structure of CuPc
broad absorption spectra in visible and partly in ultraviolet and
infrared wavelength regimes (Forrest and Xue, 2004).
Fabrication
Thin films of CuPc were deposited from a 5 wt. per cent
solution in benzene at normal (1 g) and at high (70 g)
gravity conditions. At 1 g, the films were deposited by
drop-casting, whereas at 70 g, the films were deposited
using a table-top centrifugation apparatus (Model:
HETTICH EBA-20 S). The acceleration (a) was calculated
using equation (1) as follows:
a R2 (1)
where R is the radius and is the angular velocity.
Figure 2 shows the schematic diagram of the sample. Using
the vacuum thermal evaporation technique, 200-nm thick Cu
films were deposited. The CuPc powder was dissolved in
benzene at room temperature. Glass substrates with
pre-deposited Cu electrodes having inter-electrode spacing
30-40 m were placed inside a glass tube mounted in the
centrifugal machine. The diameter and length of the glass tube
were 12 and 95 mm, respectively. During deposition of the
films, the centrifugal machine speed was set at 5,000 rpm. For
each experiment, two symmetrically installed glass tubes filled
with the solution of equal volume of 0.5 ml were used. During
the centrifugation process, the solution was allowed to
evaporate at room temperature and atmospheric pressure
without any additional heating. The process of film deposition
was completed in 30-50 min, and the thickness of the films
varied from 6 to 12 m. Impedance and capacitance
measurements of the fabricated devices were carried out using
LCR meter MT 4090 configured at 1 kHz and 1 V. The
in-situ humidity was measured using humidity/temperature
meter TECPEL 322.
Results and discussion
Figure 3 shows atomic force microscope (AFM) images of
the CuPc films deposited at normal (1 g) and high
(70 g) gravity conditions. The figure clearly shows that
films grown at 70 g offered smoother surface morphology
than films grown at 1 g. Impedance humidity and
capacitance humidity relationships for CuPc films
deposited at 1 g and 70 g are shown in Figure 4(a) and
(b), respectively. Experimental results presented in Figure 4
show that films deposited at 1 g exhibited a maximum of
45.4 per cent (Z 100 per cent/Z) change in its impedance
value, whereas in capacitance, the maximum observed
 Effect of humidity on copper phthalocyanine films Pigment & Resin Technology
Khasan S. Karimov et al. Volume 46 Number 1 2017 64 70

Figure 2 Schematic diagrams of the sample

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Figure 3 AFM images of the CuPc films deposited from the

benzene solution

Figure 4 Impedance humidity and capacitance humidity

relationships of CuPc films
3.2
65
3.1
60
3.0
Impedance

Capacitance (pF)
Impedance (M)

55 Capacitance 2.9

50 2.8

45 2.7

2.6
40
2.5
35
2.4
30 40 50 60 70 80 90 100
Relative Humidity (%)
(a)

70 2.8

65
2.7
60
Capacitance (pF)
Impedance (M)

Impedance
change was 26.5 per cent (C 100 per cent/C). On the 55 Capacitance
2.6
other hand, films deposited at 70 g showed 42.2 and 15.7
50
per cent maximum change in their impedance and
45 2.5
capacitance values, respectively.
The impedance (Z) of the samples can be represented by the 40
parallel combination of a resistor (R) and a capacitor (C). 2.4
35
From circuit point of view, the magnitude of Z caused by 30 40 50 60 70 80 90 100

Relative Humidity (%)

sample resistance and capacitance can be represented as
follows (Dally et al., 1993): (b)

R Notes: (a) Deposited at 1 g; (b) deposited at

Z (2) 70 g
(1 jRC)

66
 Effect of humidity on copper phthalocyanine films Pigment & Resin Technology
Khasan S. Karimov et al. Volume 46 Number 1 2017 64 70

Variation in impedance because of the varying values of
ambient humidity can be associated with adsorption and
absorption of water molecules by the CuPc films. As a result
of these processes, permittivity of the organic material
increases, this in return increases the capacitance of the films,
as shown in Figure 4(a) and (b). At the same time, because of
the displacement currents related to the movement of bound
charges of water molecules, the resistance of the samples may
decrease. Finally, as per equation (2), the impedance of the
samples decreases because of the increase of the capacitance
and decrease of resistance as a function of ambient humidity
as observed experimentally.
It is a well-known fact that the value of the capacitance
depends on the polarizability of the material, which has several
basic sources, that is dipolar dip, ionic i, and electronic e
polarizability (Omar, 2002). In this case, dip seems to play a
dominating role because of the presence of water dipoles
absorbed by CuPc, whereas e is an universal phenomenon
and arises because of the relative displacement of the orbital
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where CH represents the capacitance under humid condition
and Cn represents capacitance at normal conditions. RH
represents a change in relative humidity (RH HH0;
initial relative humidity H0 32 per cent) and k is a humidity
capacitive factor. For CuPc, the relative permittivity is
assumed to be 4 (Yan et al., 2010). The value of k determined
by the above expression at RH 66 per cent and Nnn was
determined from equation (3). At maximum humidity,
experimental value of CH/Cn was equated to the theoretical
value and it was found that k 0.0858.
Figure 5 shows the comparison of experimental and
simulated capacitance versus relative humidity for CuPc
samples fabricated at 1 g and 70 g. It can be seen from the
figure that the simulated data comply, with a reasonable
accuracy, to the experimental characteristics.
For simulation of relative impedance vs humidity
characteristics, we have proposed a simplified expression as
given below:
ZZ Exp HH

2
(5)
electrons. It is also assumed that CuPc molecules, after 0 0
interacting with water molecules, may form charge-transfer
complexes which as a result originate i. Thus, the total where is a fitting variable. The simulated impedance
polarizability which could affect the electrical response of humidity relationship in comparison with the experimental
CuPc films would be the sum of all the three components results is shown in Figure 6.
discussed hitherto. The simulated capacitance and impedance results both for
It is assumed that the dielectric permittivity of the CuPc 1 g and 70 g samples offer reasonable conformity to the
increases because of adsorption and absorption of water experimental data, as evident from Figures 5 and 6. The
molecules, which have a higher dielectric permittivity value. The
Figure 5 Comparison of relative experimental and simulated
absorption takes place by the diffusion process through the
capacitance of the CuPc films deposited at 1 g and 70 g with
surface of the CuPc films. This increases the capacitance value of
respect to relative humidity
the sample. Further, the presence of displacement current caused
by the water molecules could also be a source of increased 1.25
Experimental 1g
capacitance and decreased resistance values. Moreover, there is Simulated 1g
Normalized Capacitance

1.20 Experimental 70g

also a possibility of CuPc films doping by the absorbed water
Simulated 70g
molecules which as a result will increase the polarizability as well 1.15
as the concentration of free charges. Both the processes, in
1.10
return, will enhance the capacitance on one hand and decrease
the resistance of the sample on the other hand (Boguslavsky et al., 1.05
1968). For organic semiconductor humidity sensors,
1.00
impedance humidity and capacitance humidity characteristics
were simulated by Saeed et al. (2010). Their simulation was 30 40 50 60 70 80 90 100
Relative Humidity (%)
based on ClausiusMossotti relationship (Omar, 2002):

1 Nnn Figure 6 Comparison of relative experimental and simulated

(3)
2 3 impedance of the CuPc films deposited at 1 g and 70 g with
respect to relative humidity
where is the relative permittivity, Nn is the concentration of
water molecules at normal conditions, n is the polarizability 1.0

of CuPc due to absorption of water molecules at usual

Normalized Impedance

conditions and o is the permittivity of free space. Considering 0.9

the proportionality of capacitance with permittivity, we can

0.8
use the expression presented in Shah et al. (2008), Ahmad
Experimental 1g
et al. (2008) and Saeed et al. (2010): 0.7 Simulated 1g

Experimental 70g
2Nnn(1 kRH) 0.6 Simulated 70g
1
CH 30


(4) 0.5
Cn Nnn(1 kRH) 30 40 50 60 70 80 90 100
1
30 Relative humidity (%)

67
 Effect of humidity on copper phthalocyanine films
Khasan S. Karimov et al.
discrepancy in the observed and simulated data of Figures 5
and 6 could be associated with the fact that films grown at
different gravity conditions may have different structures and
compositions with varying percentage of solvent molecules.
Sensitivity (S) of CuPc-based humidity sensors can be
assessed using the following equations (Dally et al., 1993):
Z
S(Z) (6)
RH
C
S(C) (7)
RH
where Z, C and RH are the changes in impedance,
capacitance and relative humidity, respectively.
Table I shows the maximum average values of S(Z) and
S(C) for CuPc samples deposited at 1 g and 70 g. It is
evident from Table I that CuPc films deposited at high gravity
are less sensitive to the varied humidity conditions as
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compared to the films deposited at 1 g.
Presently, researchers are working not only in the area of
high gravity processing of semiconductor materials but also in
microgravity-based fabrication. In the study by Parfeniev et al.
(2001), the properties of tellurium, TeSe and Te80Si20
crystals grown under microgravity level and up to 10 g were
discussed. In general, the gravity conditions have an influence
on defects distribution, conductivity and Hall effect mobility
of the grown film.
Conclusions
CuPc thin films were deposited at different gravity conditions
(1 g and 70 g) from a solution in benzene by using
drop-casting and centrifugation. Variation in impedance and
capacitance as a function of ambient humidity levels was
assessed. It was noted that impedance of CuPc thin films
decreases, whereas their capacitance increases with increasing
values of ambient humidity. Samples fabricated at 1 g
exhibited a maximum change of 45.4 and 26.5 per cent in
their impedance and capacitance values, respectively, whereas
samples grown at 70 g demonstrated a maximum change of
42.2 and 15.7 per cent in their impedance and capacitance
values, respectively. The observed response was also
simulated, and a plausible explanation was presented. It was
demonstrated that the humidity-dependent electrical
performance could be associated both with increased
polarization and increased doping concentration caused by
absorbed water molecules. It was further shown that CuPc
films can potentially be used as a humidity-sensing material
whose sensitivity would be dependent on the chosen
fabrication parameters.
Table I Impedance S (Z) and capacitance S (C) sensitivities of the CuPc
samples deposited at 1 g and 70 g
No. Semiconductor Deposition S (Z), M/% S (C), pF%
1. CuPc 1g 0.441 0.010
2. CuPc 70 g 0.421 0.005
68
Pigment & Resin Technology
Volume 46 Number 1 2017 64 70
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Instrumentation for Engineering Measurements, Second
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Farooq, A., Karimov, K.H.S., Ahmed, N. and Usman, M.
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About the authors
Khasan S. Karimov is a Foreign Professor at the Faculty
of Electronic Engineering of GIK Institute, Pakistan. He
received his Doctor of Physical Mathematical Sciences
degree from the Department of Heat Physics, Tashkent,
Uzbekistan, 1994, and a PhD from the Physical Technical
Institute, S.-Peterburg, USSR, 1982. He received his
Engineering degree at the Electrotechnical Institute of
Communication, Tashkent, USSR, 1971. His research
projects comprised microhydropower plant, photovoltaic
system, solar biogas digester (funded by Pakistan Science
Foundation), investigation of electrical properties of
organic semiconductor sensors (funded by Higher
Education Commission of Pakistan), biogas digester,
micro-hydropower plant, micro-hydropower plant (funded
by NGO, Almaty) and solar energy utilization (funded by
69
Pigment & Resin Technology
Volume 46 Number 1 2017 64 70
ISESCO). His research interests include electrophysical
properties of organic semiconductors, organic
semiconductor devices (sensors and solar cells), materials
processing at high gravity conditions (thin films) and use of
renewable energy resources. He is a member of the Inventor
of USSR, Member of the Society of Tajikistan Inventors,
Expert of Tajikistan Academy of Sciences on Renewable
Energy Resources, Laureate of Tajikistan Academy of
Sciences Prize, 1980, Laureate of Competition Best
Inventor 1997 in Tajikistan, IEEE.
Zubair Ahmad works as a Researcher at Center for
Advanced Materials (CAM), Qatar University, Doha, Qatar.
He received his MS degree (Engineering Sciences) in 2008
from Ghulam Ishaq Khan Institute of Engineering Sciences
and Technology, Pakistan, and PhD degree (Applied Physics)
in 2011 from the same institute. His current research interests
are renewable energy-materials besides organic non-volatile
memories, organic sensors and organic smart materials.
Zubair Ahmad is the corresponding author and can be
contacted at: zubairtarar@qu.edu.qa
Noshin Fatima is a full-time PhD student in Electronics
Engineering at Muhammad Ali Jinah University, Islamabad,
Pakistan. She has done her Masters in Electronics Engineering
from Ghulam Ishaq Khan Institute, Topi, Swabi, KPK,
Pakistan. She earned BS in Electronics Engineering from
Comsats Institute Abbotabad, KPK, Pakistan. She has
published journal and conference papers. She had done
research projects with Khasan S. Karimov (in Masters and
PhD) and Muhammad Mansoor Ahmed (in PhD) on high
gravity depositions, electrochemical cells and sensors. Her
research interests include electrophysical properties of organic
semiconductors, organic semiconductor devices (sensors and
solar cells), materials processing at high gravity conditions
(thin films), use of renewable energy resources and making
cheap devices. She is a member of PEC. She earned a PEC
merit-based scholarship at the Masters level and now a PhD
scholarship from Muhammad Ali Jinnah University,
Islamabad.
Muhammad Mansoor Ahmed received his PhD degree in
Microelectronics from the University of Cambridge, UK. He
has been associated with academia at various levels for the past
20 years and, currently, is a professor in the Department of
Electronic Engineering at Mohammad Ali Jinnah University,
Islamabad, where he is also holding the post of Executive Vice
President of the University. He is a chartered engineer from
UK and also a fellow of Institution of Engineering and
Technology, UK. He was awarded the title of European
Engineer (Eur. Ing). in 2002 by the European Federation. He
is a senior member of the Institution of Electrical and
Electronic Engineering, USA. He enjoys lifetime membership
of IEEE Electron Devices and IEEE Microwave Theory and
Technique societies, USA. He has authored more than 100
research papers in the field of microelectronics, microwave
MESFETs and HEMTs, Electromagnetics and RF
Engineering. His ISI research impact factor is 50 with H &
i10 factors 13 and 18, respectively. He has more than 540
research citations, and based on his research contributions, he
was awarded a gold medal in the field of Engineering and
 Effect of humidity on copper phthalocyanine films
Khasan S. Karimov et al.
Technology by the Pakistan Academy of Sciences in 2008. He
holds the IEEE technical activities chair and has rendered
services as an organizer, session and general chairs of several
IEEE International Conferences.
Muhammad Abid is a Professor and the Director of
Interdisciplinary Research Center at COMSATS Institute of
Information Technology, Pakistan. His research interests
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Pigment & Resin Technology
Volume 46 Number 1 2017 64 70
include renewable energy systems, water and sediment flow
simulations, welding simulations, bolted flanged pipe joints,
product design and optimization and structural design
engineering. He has been awarded the Pakistan Academy of
Sciences Gold Medal, Best Researcher and Best Teacher
Award by HCE Pakistan, Best Research Award by IMechE
and several others.