International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329

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International Journal of Lightweight Materials and Manufacture

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Original Article

Fabrication of PEDOT: PSS conductive patterns on photo paper

substrate through electro-hydrodynamic jet printing process
Umer Farooq a, Imran Khan a, Salman Ahmad b, Muhammad Abas c,
Muhammad Alam Zaib Khan a, Khalid Rahman b, *
a
Department of Mechanical Engineering, University of Engineering and Technology, Peshawar, KPK, 25120, Pakistan
b
Faculty of Mechanical Engineering, GIK Institute of Engineering Sciences and Technology, Topi, KPK, 23640, Pakistan
c
Department of Industrial Engineering, University of Engineering and Technology, Peshawar, KPK, 25000, Pakistan

a r t i c l e i n f o a b s t r a c t

Article history: Conductive polymers such as PEDOT: PSS have gained popularity in sensor fabrication and integration. The
Received 10 June 2019 objective of current work is to investigate the effects of process parameters on the final quality of
Received in revised form conductive patterns fabricated through electro-hydrodynamic (EHD) jet printing. Solutions of different
22 June 2019
concentration of PEDOT: PSS in ethylene glycol and isopropyl alcohol were prepared for printing purpose.
Accepted 24 June 2019
Available online 28 June 2019
Effects of operating parameters such as voltage, frequency, pressure and printing speed on quality of
printing patterns were experimentally investigated. Solution with higher concentration of PEDOT: PSS in
ethylene glycol has shown better jetting stability even at higher frequencies and printing speeds. Increasing
Keywords:
Electro-hydrodynamic (EHD) jet printing
the frequency at high printing speed reduced the size of pattern width. Similarly, higher pulse voltage in the
PEDOT: PSS working envelope also reduced the pattern size. However, increasing the pressure increased the size of
Photo paper substrate width of pattern. A drastic decrease in the pattern width was observed with increase in printing speed. A
Pattern width pattern width of approximately 19.6 mm was produced at 500 Hz of frequency and 2000 mm/min of
Conductive patterns printing speed, the electrical resistance of which is 1.03
106 U/mm. Finally, these results were compared
with the same concentration of PEDOT: PSS in isopropyl alcohol reported in previous studies.
© 2019 The Authors. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-
nc-nd/4.0/).

1. Introduction electromechanical systems (MEMS) and other application has been

In present era of nano and micro technology every electronic
device is getting smaller in size and efficient in performance.
Different patterning technologies have been opted by electronic in-
dustries to get the desired results. Numerous research works have
been done to apply printing techniques to electronic manufacturing
systems on a commercial scale [1e3]. In recent years flexible printed
electronics has gone a new level requiring new techniques of print-
ing. Electro-hydrodynamic (EHD) jet printing is a novel technique in
the field of printed electronics to produce fine resolution patterns [4].
Electronics like printed circuit board, sensors, displays, micro-
* Corresponding author.
E-mail addresses: umer5764@gmail.com (U. Farooq), engrimran@uetpeshawar.
edu.pk (I. Khan), salmanahmad@gmail.com (S. Ahmad), gh_ghumman@hotmail.
com (M. Abas), muhammadabas@uetpeshawar.edu.pk (M.A. Zaib Khan),
khalidrah@gmail.com (K. Rahman).
Peer review under responsibility of Editorial Board of International Journal of
Lightweight Materials and Manufacture.
the main focus of printed electronics [5e7].
Electro-hydrodynamic jet printing (EHD) printing or patterning
is accomplished by applying high potential (voltage) at the tip of
capillary to form a cone jet from the meniscus [8]. In EHD printing
the fluid is pressurized to form a meniscus at the tip of a capillary
then electric field is applied to transform that convex meniscus into
cone jet by balancing Surface tension force and electrostatic force
[9]. When electric field is applied between the nozzle and substrate,
charges start to accumulate at the tip of nozzle inducing Maxwell
electrical stresses causing convex meniscus to deform into cone
[10]. As the electrostatic force increases and exceeds the fluid sur-
face tension force a thin jet is emerged from the cone as known as
cone-jet. For any liquid cone-jet diameter depends on applied
voltage, flow rate and nozzle diameter. EHD jet printing can be
continuous or drop-on-demand (DOD) mode depending upon the
application of Electrical force [11]. EHD jetting can produce a wide
angle spray, discrete drops and continuous stream depending
amplitude, duration and static biasing field of the pulse [12].

https://doi.org/10.1016/j.ijlmm.2019.06.002
2588-8404/© 2019 The Authors. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the CC BY-NC-ND
license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329 319

PEODT: PSS is a conductive polymer and it has gained its
popularity in the field of printed electronics due to better optical
transparency, excellent stability and high electrical conductivity
[13,14]. PEDOT: PSS has countless application; it can be used in
many electronic devices like sensors, LEDs, thin-film transistors and
photovoltaics [15e17]. Although different conventional techniques
like photolithography is well known techniques for producing
patterns on micro-scale, yet it cannot be successfully applied to
pattern PEDOT: PSS [18]. The processes carried out to pattern
PEDOT: PSS through photolithography actually damages the layers
of PEODT: PSS [19]. So a new technique was needed to pattern
PEDOT: PSS. Sooman et al. [20] has printed PEDOT: PSS through
EHD jet to check the effect of non-ionic surfactant. Cone jet was
confirmed and different parameters like applied voltage, working
distance and flow rate were varied and adjusted to get the desired
patterns. Navanneethan et al. [21] deposited PEDOT: PSS through
EHD atomization (EHDA) to produce thin films.
This investigation presents the drop-on-demand EHD printing
of PEDOT: PSS solution by dissolving it in ethylene glycol and iso-
propyl alcohol on a flexible photo paper substrate. Different solu-
tions based on concentration by weight were produced and their
parametric study was carried out. Optical microscopy was carried
out to measure the pattern. These patterns has potential applica-
tions in flexible sensors fabrication.
particular setup the high voltage system was devised by connecting
Matsusada high voltage amplifier. Model: AMT-5B20 with a Levell
type TG 302 function generator to produce different types of sig-
nals. These signals were then monitored through a GWINSTEK GDS-
1102A-U Oscilloscope.
Liquid containing and supply system comprises of 5cc syringe,
to which 100 mm (inner diameter) metallic nozzle was attached. A
pipe from air compressor was connected to nozzle for maintaining
the meniscus at the tip of nozzle. Monitoring system consists of
Plunix TM-200 camera which was connected to a laptop for
monitoring the entire process. For substrate positioning system
Triac Fanuc ATC CNC machine was used.
2.4. Characterization techniques
Electrical characterization was done by purposely build 2-point
probe apparatus (with measurement error ± 1%) as show in the
Fig. 2a. Two methods can be followed: i) voltage divider technique,
the voltage across the known resistance is measured using digital
multi-meter (DMM). Using formula unknown resistance is found
out [22].
 
R1
Vout ¼ Vcc
R 1 þ R2

2. Materials and methods
2.1. Materials
Commercially available PEDOT: PSS was dissolved in ethylene
glycol (EG) and isopropyl alcohol (IPA 99.0% pure). Commercially
available photographic paper is used as substrate. Conductive silver
paste for making connections to measure resistance was purchased
from Chemetronics®.
where R1 is known resistance, R2 is the resistance of pattern, Vcc is
the output voltage of power supply and Vout is the voltage across
known resistor as shown Fig. 2b. ii) 2-point probe technique, the
current is allowed to pass through the pattern and values of current
and voltage is measured to plot IV curve.
Pattern size was measure using optical microscopy and TESCAN
Vega 3 scanning electron microscope (SEM). Inks viscosities and
surface tensions were measured using viscometer and stalag-
mometer, respectively.

2.2. Ink preparation 3. Results and discussion

PEDOT: PSS was dissolved in ethylene glycol (EG) and isopropyl
alcohol (IPA) for EHD jet printing. PEDOT: PSS and solvent (EG or
IPA) were then mixed by a vortex mixer for 5e10 min. After that
they were stirred for 50 min in magnetic stirrer at 1500 rpm. Finally
the solutions were filtered through a PTFE. 2 mm in order to get
homogenous solutions.
Four different concentrations of PEDOT: PSS were prepared.
Properties of each solution were measured. Details of each solution
is given in Table 1. After printing, the patterns were cured at 110  C
for 50 min in dry oven.
2.3. Experimental setup
3.1. Operating envelop
To study the effect of parameters on jetting process and patterns
produced working envelops should be known and understood. In
this study four Inks of different composition were used so four
working envelops were studied. Working envelops shows the range
in which the stable cone jet is achieved as shown in Fig. 3. Solution
A produces stable cone-jet in range of 1.6e2.1 kV at 1 psi, solution B
produces stable cone jet in 1.7e2.18 kV at 1 psi, stable cone-jet in
solution C ranges from 1.85 to 2.2 kV at 1 psi while solution D has
stable cone jet between 1.58 kV and 1.96 kV at 1 psi. These varia-
tions in voltage ranges are discussed in coming sections.

The EHD jet printing setup consists of four sub system i.e. high 3.2. Effects of voltage
voltage system, liquid supply and containing system, monitoring
system and substrate positioning system as shown in Fig. 1. In this Voltage has its effects on jetting phenomenon as well as on the
pattern size. Increase in voltage will decrease the pattern size as the
voltage is increased the increase in electrical forces occur. Electrical
Table 1
Physical properties of Solutions. forces combined with gravitational forces acts on the cone and
results in a detachment of small droplet. In drop-on-demand we
Composition Designation Viscosity (cP) Surface tension (dyn/cm)
have a base voltage (Vb) and a pulse voltage (Vp). Base voltage
1/2 (w/w) ratio Solution A 87.67 50.19 maintains the cone while pulse voltage eject droplet from the cone.
PEDOT: PSS in EG
The difference between base and pulse voltage also affect the
1/1 (w/w) ratio Solution B 155.89 65.7
PEDOT: PSS in EG jetting phenomenon as can be observed by Fig. 4.
2/1 (w/w) ratio Solution C 380.79 88.3 In Fig. 4 the graph represents the working envelop of solution A.
PEDOT: PSS in EG In the graph there two curves in between these two curves we have
2/1 (w/w) ratio Solution D 120.83 15.2 stable cone-jet. Below 1st curve dripping and micro-dripping oc-
PEDOT: PSS in IPA
curs, while above 2nd curve multi jet and complex jetting occurs.
320 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329

Fig. 1. (a) Actual experimental setup (b) Schematic of the experimental setup.

Fig. 2. (a) Purposely build apparatus for electrical characterization. (b) Electrical circuit produced to find the value of resistance of patterns.
 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329 321

Fig. 3. Working envelop of (a) solution A, (b) solution B, (c) solution C and (d) solution D.

Now in order to produce a drop-on-demand the base voltage
should be below the initiation curve and pulse voltage should be in
between the two curves. In graph four different points Vb1, Vb2, Vp1,
and Vp2 having value of 1.2 kV, 1.3 kV, 1.57 kV and 1.63 kV respec-
tively. These values were selected in order to understand the effect
of voltage that was observed practically. A couple of cases have
been studied to completely understand the effect of voltage on
jetting phenomenon.
In first case Vb1 was set as base voltage and Vp2 as pulse
voltage. As it can be observed that the difference between both
voltages are on the higher side, which translate into higher
movement in the meniscus. Vb1 is far below the stable cone jet
initiation, while Vp2 is closer to cone-jet ending curve. In this
particular case once the pulse voltage is applied first the partially
deformed meniscus is deformed into a cone-jet and then it ejects
the droplet. This results in a high movement of meniscus. This
might result in an unstable drop-on-demand and irregular
pattern as shown in the Fig. 5a.
In second case Vb2 which is quite close to the 1st curve thus
resulting in a cone shape deformed from meniscus. At this stage no
ejection of droplet takes place but as the pulse voltage is applied
(could be Vp1 or Vp2) a small detachment from the cone-jet. This
results in a fine, regular pattern with clear edges as shown in the
Fig. 5b.
322 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329

Fig. 4. Working envelope of Solution A.

Fig. 5. Effect of voltage of jetting (a) first case: base voltage is lower than stable cone-jet initiation, (b) second case: base voltage is quite close to the stable cone-jet initiation.

As discussed earlier the increment in voltage also affects the

pattern size. To verify that a couple case from the same graph
have been studied. In both cases Vb2 was set as base voltage
while in first case Vp1 was set to be the pulse voltage while in
second case Vp2 was pulse voltage. As Vp2 is greater than Vp1,
thus a small volume detachment takes place in second case. In
both case a stable jet was observed due to minimal movement
of meniscus. The difference is pattern size can be observed from
the following Fig. 6. These patterns were produced under similar
conditions the only difference was in the application of pulse
voltage Vp.

3.3. Effects of frequency

The relation between frequency and pattern size is mainly

dependent on printing speed. At lower printing (25 mm/min)
speeds if the frequency is high, an increase in the pattern width will
be observed. At higher printing (750 mm/min), a decrease in the
pattern size was observed this could be confirmed from the graph
shown in Fig. 7.
Although at higher frequency, the volume of the drop ejecting Fig. 6. Digital microscopic images of patterns showing the effect of pulse voltage (a)
from the cone decreases. This is mainly because of the charge first case (b) second case.
 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329 323

Fig. 7. Variation of Pattern width with frequency (a) 25 mm/min (b) 750 mm/min.

accumulation time. Higher the frequency less time will be available
for the charge to accumulate thus resulting in a smaller volume
detachment. Similarly at lower frequencies more time is available
for charge accumulation which may lead to large volume detach-
ment from the cone. In the graph curve of printing speed 25 mm/
min portrays an opposite result. This may be due to the percent
overlap of droplet because as the frequency is increased the drop-
lets detachment rate also increases. A pattern printed at a fre-
quency of 10 Hz with printing speed of 25 mm/min means that in
0.42 mm 10 drops will be deposited. If the frequency is raised up to
100 Hz then 100 drops will be deposited over length of 0.42 mm.
This cause percent overlap of droplets to increase even though the
volume ejected from cone-jet will be low yet an increase in the
pattern width will occur. The effect of frequency can be seen in the
Figs. 7 and 8. In Fig. 7b the curve of printing speed 750 mm/min
shows a decrease in the pattern width with increase in the fre-
quency. This could also be confirmed from the microscopic images
of patterns in Fig. 8.
3.4. Effects of substrate speed
Substrate speed has a great effect on the size of pattern. With
increase in the substrate speed, the width of pattern decreases. The
droplets coming out of nozzle at a particular frequency needs to be
deposited over the substrate if the printing speed is low the
droplets will overlap each other such that the pattern size would
increase. If this overlap is more than 50% the droplets tends to
expand causing an increase in the overall pattern width. If the

Fig. 8. Microscopic images of patterns showing combine effects of Frequency and printing speed (a) Variation in Pattern width with frequency at printing speed of 25 mm/min (b) at
750 mm/min.
324 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329

Fig. 9. Variation of pattern width with substrate speed of all four solutions.

overlap is equal to 50%, the diameter of droplet and pattern are
almost the same. Lower than 50% overlap may result in irregular
pattern. The variable size of pattern width of each solution is shown
in Fig. 9.
It can be seen that pattern width of almost all of the solutions
varies with printing speed in similar fashion with minor variation
from each other. Probable reason could be effect of viscosity of
surface tension difference. Solution A, B and C has an increase in the
viscosity so the pattern width increases in the same fashion. In case
of solution D also it has lower surface tension which caused the
deposited droplet to expand on the substrate therefore an increase
in the pattern width was noticed. Variation in pattern can also be
seen in the Fig. 10. All the patterns shown were printed on constant
frequency of 10 Hz. The voltage requirement for each solution was
different due to variation in physical properties. For solution A base
voltage was 1.3 kV while pulse voltage 1.67 kV at 0.6 psi. Similarly

Fig. 10. Microscopic images of patterns showing variation in width with increase in substrate speed i.e 25 mm/min, 50 mm/min, 100 mm/min and 200 mm/min (patterns from left
to right) (a) solution A (b) solution B from (c) solution C (d) solution D.
 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329 325

for solution B, C and D voltage requirements were 1.5 kV base and
1.75 kV pulse voltage at 0.8 psi, 1.87 kV base and 2.1 kV pulse
voltage and 1.4 kV base and 1.6 kV pulse T 0.75 psi, respectively.
3.5. Effects of pressure
A pressure has maintained at the back of ink supplied at nozzle
to control the flow rate of the ink. Increment in pressure forces
more fluid to eject from the capillary. More fluid ejection increases
the voltage requirement. At high pressure more fluid is present at
the tip of nozzle forming a large meniscus thus more voltage is
required to deform larger meniscus as compared to smaller one.
The effect of pressure on voltage requirement can be summarized
in the Fig. 11 as shown.
It can be observed that the voltage requirement increases with
increase in the back pressure. All four solutions show the same
behavior. Requirement of voltage for different solution has varied.
For solution C the voltage requirement is more than A, B and D
reason for that is Surface tension. Solution D has the lowest surface
tension of all, thus requiring low voltage to form a cone-jet.
The pressure also affects pattern width. With increase in pres-
sure the pattern width also increased. As the flow rate is increased
more volume will start ejecting from the nozzle, even at application
of a very high voltage the volume deposited on substrate will be
more than that of low flow rate. Because the cone jet form by larger
meniscus will eject more volume than that of smaller meniscus.
The patterns of solution A at pressure of 1.5 and 0.75 psi are shown
in the Fig. 12.
The flow rate should also match the frequency. If the flow rate is
increased higher mass of ink will be present at tip of nozzle. The
mass should detach the cone as soon as possible to leave empty
space for the incoming liquid. Improper match of frequency and
flow rate might result in an irregular pattern. Fig. 13 confirms this
situation.
All solutions have shown same behavior to change in flow rate.
In Fig. 13, both patterns were drawn at 50 Hz at different pressure
level of 2 and 0.75 psi. At 2 psi the flow rate was high so, the fre-
quency did not synchronized with flow rate resulting in an irreg-
ular pattern and large pattern width. The meniscus formed is also
difficult to deform into a proper cone. However, at 0.75 psi the

Fig. 11. Relationship of Voltage with pressure for various solutions.

Fig. 12. Increase in the size of pattern width with pressure (a) solution A at 1.5 psi (b) solution A at 0.75 psi.
326 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329
Fig. 13. Effect of pressure on jetting Phenomenon (a) jetting at 2 psi for solution A
(high mass flow rate), (b) jetting at 0.75 psi for solution A (adequate mass flow rate).
frequency did match the flow rate. A proper cone jet with small
width regular pattern was produced as shown in Fig. 13.
3.6. Effects of viscosity and surface tension
Viscosity and surface tension has greatly affected the jetting
phenomenon as well as the pattern size. Increase in viscosity in-
creases the pattern size or diameter of droplet. In order to study this
behavior the droplets of different solution were produce under
similar operating conditions. A clear increase in deposited droplet
diameter was observed with increase in viscosity this is mainly due
to reduction in charge mobility. The graph plotted in Fig. 14
Fig. 14. Variation of droplet diameter with viscosity.
confirms the above results. The droplets of different solutions can
be seen in the Fig. 15 as well.
Solution A with lower viscosity has smaller droplet diameter as
compared to other solutions. Solution C with highest viscosity of-
fers higher droplet diameter but in turn the jet produced by solu-
tion C was more stable than other solutions. The effect of surface
tension is also portrayed by figure. The droplet produced by Solu-
tion C has definite edges as compared to solution A and D because
solution C has the highest surface tension. At higher frequencies
and feed rates the process of droplet production and deposition
increases but the volume ejecting from the cone decreases so the
deposited pattern should have definite edges. In this case, pattern
produced from solution has clear edges due to higher surface ten-
sion. Although the size of pattern width is more than that of solu-
tion A, B and D. As shown in the Fig. 16.
3.7. Effects of variations in concentrations on resistance
Variations in concentrations of different solutions have their
effects on resistance offering. Apparently solution with more con-
tent of PEDOT: PSS will offer less resistance as compared to others.
Out of these four solutions, solution C has the highest content of
PEDOT: PSS, which is 200% by weight in ethylene glycol. Solution D
is also a 200% by weight solution but it is dissolved in isopropyl
alcohol. The IV curves of all four solutions have been plotted in
Fig. 17 as shown.
All of the curves were produced from the pattern of same width.
The slope of IV curve gives the value of resistance. It can be seen
that solution C has the lowest slope which means that it offer less
resistance as compared to other. The reason for this is content of
PEDOT: PSS available in the solution. Solution D also comprises of
200% of PEDOT: PSS in IPA by weight but still its resistance was
reported on the higher side because the density of IPA is less than
that of ethylene glycol so which means that solution C will have
more content of PEDOT: PSS. This is why solution C offers lowest
resistance. The variation in resistance with pattern width of each
solution is also shown in Fig. 18.
The logarithmic graph portrays a linear variation for solution A
and B. Solution C and D has a few ups and downs and does not
 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329 327

Fig. 15. Optical microscopic images droplets of solutions with different viscosities (a) solution A, (b) solution D, (c) solution B, (d) solution C.

follow a linear behavior completely. This graph also proves that different solutions were produced under similar conditions. Pat-
solution C offers quite less resistance as compared to other solu- terns were produced at 100 Hz of frequency with respective
tions. Parameters like frequency and printing speed also affect the required voltages at different feed rates ranging from 25 mm/min
resistance as discussed earlier, and for this, the patterns of to 900 mm/min.

Fig. 16. Optical microscopic images of patterns produced from (a) solution A, (b) solution D, (c) solution B and (d) solution C.
328 U. Farooq et al. / International Journal of Lightweight Materials and Manufacture 2 (2019) 318e329
Fig. 17. IV curve of various solutions.
Fig. 18. Logarithmic graph of pattern width vs resistance.
4. Conclusions
In this study, conductive patterns were successfully fabricated
using drop-on-demand EHD technique with ethylene glycol,
PEDOT: PSS and paper as solvent, solute and substrate respectively.
The patterns were fabricated by varying the process parameters. It
can be concluded that all the process parameters affected the final
quality of conductive patterns such as continuity of conductive
patterns, width and resistance etc. Increase in the frequency at high
printing speed reduced the size of pattern width. Pulse voltage
higher in the working envelope between two limits of Cone-jet also
reduced the pattern size. Increase in the pressure also increased the
size of pattern width. A drastic decrease in the size of pattern width
was observed with increment in printing speed. With the variation
of concentrations, viscosity of solutions was varied which in turn
affected the jetting and pattern size. Solution C offered less resis-
tance as compared to other solutions. Controlled EHD Jetting at
high feed rate and frequency was also observed in the solution C.
This research is aimed at producing patterns of PEDOT: PSS smaller
than the inner diameter of nozzle through electro-hydrodynamic
jet printing and this aim has been achieved. A pattern size of
19.6 mm was produced from 100 mm inner diameter nozzle at
500 Hz, 2000 mm/min, 1.7 psi, base voltage 1.83 and pulse voltage
2.1 and working distance of 1 mm using solution C.
Funding
This research received no external funding.
Conflicts of interest
The authors declare no conflict of interest. The funders had no
role in the design of the study; in the collection, analyses, or
interpretation of data; in the writing of the manuscript, or in the
decision to publish the results.
Acknowledgments
The authors are thankful to GIK Institute of Engineering Sciences
and Technology, Topi and University of Engineering and Technology
Peshawar for providing technical support.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.ijlmm.2019.06.002.
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