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Chemical Engineering Journal 253 (2014) 325331

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Fabrication of CdSe/ZnS quantum dots thin lm by

electrohydrodynamics atomization technique for solution based exible
hybrid OLED application
Muhammad Zubair a, Maria Mustafa a, Kangtaek Lee b, Cheolsang Yoon b, Yang Hoi Doh c,
Kyung Hyun Choi a,
Department of Mechatronics Engineering, Jeju National University, 690-756, Republic of Korea
Department of Chemical and Biomolecular Engineering, Yonsei University, 120-749, Republic of Korea
Department of Electronics Engineering, Jeju National University, 690-756, Republic of Korea

h i g h l i g h t s g r a p h i c a l a b s t r a c t

 Synthesis of core/shell CdSe/ZnS

quantum dots.
 Spray of quantum dots by
electrohydrodynamics atomization
 Fabrication of hybrid organic light
emitting diode on PET substrate.
 Characterization of hybrid organic
light emitting diode.

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

Article history: The synthesis and novel fabrication of quantum dot layers has been performed by using electrohydrody-
Received 27 February 2014 namics atomization technique. The surface, optical and electrical properties of the fabricated lms have
Received in revised form 4 May 2014 been characterized by FE-SEM, TEM, spectroscopes and semiconductor device analyzer. The CdSe/ZnS
Accepted 7 May 2014
core/shell quantum dots have been synthesized and dispersed in toluene and DMSO as cosolvents. The
Available online 24 May 2014
sprayed CdSe/ZnS quantum dots have been employed as emissive layer. The conjugate polymers of
PEDOT:PSS and MEH-PPV are used as the hole and electron transport layers. The thickness of emissive
layer for hybrid device has been optimized by changing the standoff distance of electrohydrodynamics
Electrohydrodynamics atomization
Conjugate polymers
atomization system. The exible hybrid device with optimized thickness of quantum dots showed red
Quantum dots light at 634 nm wavelength in visible range with 165 mA/cm2 current density and 2.2 lux of luminance
Hybrid light emitting diode at 15 V.
Flexible 2014 Elsevier B.V. All rights reserved.

1. Introduction polymer devices have advantages like easy fabrication, low cost,
lightweight, human friendly, sustainable raw materials, very thin,
Organic light emitting diodes (OLEDs) along with luminance large view angle, and fast response [3,4]. The solution-based
performance were rst reported in 1987 [1]. From there on a lot polymers make the fabrication process easy as compared to the
of research has been reported on OLEDs [2]. The conjugated inorganic conventional LEDs [5]. In OLEDs, usually Indium tin oxide
(ITO) coated glass is used as the transparent anode on which a hole
transport layer is casted by spin coating. On this hole transport
Corresponding author. Tel.: +82647543713; fax: +82647523174. layer, emissive layer is coated in which the holes and electrons
E-mail address: (K.H. Choi). combine and emit photon. Electron transport layer is coated on
1385-8947/ 2014 Elsevier B.V. All rights reserved.
326 M. Zubair et al. / Chemical Engineering Journal 253 (2014) 325331

top of emissive layer. Finally, the aluminum layer is thermally O/sq, cadmium oxide (CdO, 99.99%), zinc acetate (Zn(CH3COO)2
evaporated onto the electron transport layer as the reective 99.99%, powder), oleic acid(OA, 90%), trioctylphosphine (TOP,
cathode [6,7]. 90%), selenium (Se, 99.99%, powder), sulfur (S, 99.9%, powder), 1-
To enhance the emissive characteristics of OLEDs, quantum dots octadecene (90%), dodecanethiol (99%) and dimethyl sulfoxide
(QDs) have been used [810]. QDs are nanocrystal with excellent (DMSO, 99.9%) were purchased from Sigma Aldrich (South Korea).
emissive properties because of quantum connement effect [11]. PEDOT:PSS was purchased from Agfa Materials Japan. Acetone,
The narrow emission wavelength that is tunable throughout the chloroform, and isopropanol were purchased from Daejon
visible spectra, tunable band gap and solution process ability make Chemicals and Metal Co, Ltd, South Korea. All solvents were used
QDs excellent candidates in many application as emissive layers in as received.
OLEDs devices [12,13], composite materials [14], solar cells [15,16],
electroactive polymers [17] and biological imaging [11]. Since 2.2. Quantum dots ink synthesis
homogenous and uniform spray of QDs in large area is an essential
requirement in emissive devices [9], researchers have opted for CdSe/ZnS QDs were synthesized using the previously reported
dropping solution and then drying in oven [18], spin coating method with modication [34]. Briey, 2 mmol of CdO, 4 mmol
[19], spin coating with air-shear force [9] and transfer printing of Zn(CH3COO)2, 5 mL of OA were placed into 250 mL of three-neck
[20]. Still there is a need to adopt a fabrication technique that ask with vigorous stirring, and the temperature was raised to
can be deployed to produce thin lm for large area coverage. 150 C, followed by evacuation for 30 min. Then, 50 mL of
Electrohydrodynamics atomization (EHDA) is one of the easy, 1-octadecene was added, and then reactor was heated to 300 C
cost effective, and robust techniques for spraying which can be to form Cd(OA)2 and Zn(OA)2. At the elevated temperature,
applied for large area spray applications. EHDA is a single step 0.4 mL of 1 M TOPSe was rapidly injected into the reactor to pro-
spray process in which functional materials like polymer, nanopar- duce CdSe cores. After 1.5 min, 0.6 mL of dodecanethiol was added
ticles or quantum dots dissolved or dispersed in solvents are dropwise at rate of 1 mL/min, and the mixture was allowed to react
sprayed onto the substrate under the inuence of electric eld at at 300 C for 20 min under N2 atmosphere. To passivate QDs,
room temperature and atmospheric pressure [21]. A cone is formed 4 mmol of sulfur dissolved in 2 mL of TOP was added, and the reac-
at the exit of capillary by the surface tension of the solution work- tion proceeded for additional 10 min under N2 atmosphere. Then
ing against Maxwell stresses induced by the electric eld. The jet the mixture was cooled to room temperature to produce CdSe/
breaks into droplets and further disintegrates into smaller droplets ZnS core/shell QDs. For purication, chloroform and acetone were
by Coulomb forces and this continually ssion leads to micron added to the suspensions, followed by centrifugation at 7,000 rpm
sized droplets which are deposited on substrate and a uniform thin for 30 min and redispersion in toluene and DMSO cosolvent.
layer is achieved [22]. At different modes of EHDA phenomena can
be observed at different voltages. Researchers have used EHDA for 2.3. Device fabrication
spray purposes of organic and inorganic materials [2330].
Muhammad et al. [23] discussed characterization of Zinc Oxide The H-LED fabrication process and structure of device (ITO/PED-
(ZnO) sprayed by EHDA. Zirconium dioxide (ZrO2), Titanium OT:PSS/CdSe-ZnS QD/MEH-PPV/Al) is shown in Fig. 1. The ITO
dioxide (TiO2) graphene akes and graphene oxide were sprayed coated PET was initially cleaned by using acetone and then isopro-
by EHDA for memristor by Muhammad et al. [24], Maria et al. panol in bath sonicator for 15 min each. After cleaning, the ITO
[25], and Navaneethan et al. [26]. Organic polymers like poly coated PET was rinsed with deionized water and placed in oven
[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene] (MEH- to dry for 15 min. The substrate was further cleaned to remove
PPV), Poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate) any organic contamination using ultraviolet (UV) treatment for
(PEDOT:PSS), poly(3-hexylthiophene) phenyl-C61-butyric acid 60 s. Aqueous solution of PEDOT:PSS was made by in-house proce-
methyl ester (P3HT:PCBM) and Poly[(9,9-di-n-octyluorenyl-2,7- dure using water and isopropanol which was explained clearly in
diyl)-alt-(benzo[2,1,3]thiadiazol-4,8-diyl)] (F8BT) solutions were our previous work [28]. The viscosity of aqueous PEDOT:PSS solu-
sprayed by EHDA by Muhammad et al. [27], Navaneethan et al. tion was 43.5 mPa.S. PEDOT:PSS was coated on ITO coated PET
[28,29], Choi et al. [31] and Maria et al. [30] respectively. Zhu using spin coating technique with spin coating speed of 1500 rpm
et al. and Wei et al. showed that the QD in ionic liquid aided in for 30 s. The thin layer was dried at 100 C for 30 min. CdSe/ZnS
the formation of polymer nanobers by electrospinning process quantum dots of 5 wt% were dispersed in toluene with dimethyl
[32,33]. sulfoxide (DMSO) as cosolvent. The viscosity of quantum dots
In this work, cadmium selenide/zinc sulde (CdSe/ZnS) core/ solution was 0.56 mPa.S. Quantum dots were sprayed using
shell quantum dots are sprayed by electrohydrodynamic atomiza- electrohydrodynamics atomization technique. After spray, the
tion process for the fabrication of exible hybrid OLED. The photo- device was dried in oven at 110 C for 1 h. Chloroform was used
luminance and transmission electron microscope (TEM) images are to make 0.5% MEH-PPV solution with viscosity of 4.76 mPa.S.
used to nd the size and emissive wavelength of QDs. A hybrid con- MEH-PPV was deposited on the device using spin coating technique
jugate polymer OLED is fabricated which has CdSe/ZnS QDs as emis- with 1500 rpm for 30 s. The thin lm was dried at 100 C for 30 min
sive layer. ITO is used as the transparent anode, PEDOT:PSS as hole in oven afterwards. The top electrode was made by thermally
transport layer, MEH-PPV as electron transport layer and aluminum evaporated aluminum at deposition pressure of 10 6 torr and depo-
as reective cathode. Electroluminance of the fabricated device is sition rate of 3 /s. The thickness of top electrode was 100 nm with
used to conrm the functionality of atomized emissive layer. active area of 0.8  0.8 cm2. After that, an ultraviolet (UV) exible
Current voltage (IV) characterization is performed to analyze the epoxy binder was used to encapsulate the device. Initially devices
electrical performance of hybrid-light emitting diode (H-LED). were fabricated on ITO coated glass substrate for the optimization
of spray process. Once the spray process was optimized, the ITO
2. Method coated glass substrate was replaced by ITO coated PET substrate.

2.1. Materials 2.4. Electrohydrodynamics atomization setup

MEH-PPV powder (average molecular weight 40,00070,000), The setup for EHDA is shown in Fig. 2. EHDA process was carried
ITO coated Polyethylene terephthalate (PET) with resistivity of 12 out at room temperature (25 C & 50% humidity) and atmospheric
M. Zubair et al. / Chemical Engineering Journal 253 (2014) 325331 327

Fig. 1. Device Structure and fabrication process of hybrid CdSe/ZnS QDs H-LED device.

(Motion Pro X) was used to observe the EHDA phenomena illumi-

nated by a light source (Moritex MLET-A080W1LRD). The standoff
distance, which is the distance between the substrate and tip of
capillary, was changed from 10 mm to 5 mm to see the effect on
the thickness of QDs thin layer.

2.5. Characterizations

Surface morphologies of PEDOT:PSS and MEH-PPV lms were

analyzed by (FE-SEM) (JEOL JSM-7600F, Japan). This system was
operated at accelerating voltage of 5 kV. The QDs ink was analyzed
by transmission electron microscopy (TEM, JEOL JEM 2010). The
thickness of thin lm was measured by thin lm thickness measur-
ing reectometer (K-MAC ST4000-DLX). Photoluminance (PL) of
QDs ink was observed by photoluminescence spectroscopy (Perkin
Elmer LS-55) with 365 nm excitation wavelength. The optical
properties were studied using ultra violet/visible spectrometer
(Shimadzu UV-3150) within visible color range 300800 nm. The
HOMO and LUMO values of the QDs were determined from the
cyclic voltammetry (CV) for which a three electrode electrochemi-
Fig. 2. Setup of Electrohydrodynamics Atomization Technique. cal cell was used with a potentiostat (VSP, Bio-Logic). We used a
glassy carbon disk as a working electrode, a Pt wire as a counter
electrode, and a Ag/0.01 M AgNO3 + 0.1 M tetrabutylammonium
pressure. The in-house developed EHDA setup was consisted of a hexauorophosphate (TBAPF6) acetonitrile (Ag/Ag+) as a reference
metallic capillary, of internal diameter 110 lm, which was electrode. The CV measurements were made from 2.0 V to 1.7 V
attached to the nozzle adopter (NanoNC). This nozzle adopter at a scan rate of 20 mV/s.
was connected to the syringe (Hamilton, Model 1001 GASTIGHT The electrical characterization of H-LED devices was performed
syringe) placed in the infusion pump (Harward Apparatus, PHD by semiconductor device analyzer (Agilent B1500A) with current
2000 infusion). This infusion pump controlled the ow rate of resolution of 1 fA. A probe station (MST8000C) was used to place
the ink during spray process. The nozzle was attached to the the samples during electrical performance analysis. The luminance
head-holder. Its motion along x, y and z axes was guided by three of the H-LED devices was measured by lux meter (Minolta LS-100).
linear motors controlled by NI motion controller (NI-PXI-7340) The Commission International dEclairage (CIE) coordinates (x, y)
was in placed in PXI (NI-PXI-8110). An interface board were also obtained by lux meter. The electroluminance (EL) of
(CW7764YS3) was used to setup communication and control of devices was measured by calibrated spectrometer (Avantes
limit switches. A program in National Instruments LabVIEWver- AvaSpec-ULS2048 StarLine Versatile Fiber-optic).
sion 8.6 was written, which allowed the movement the
head-holder in any pattern, which can be described by lines and 3. Results and discussion
arcs. The metallic capillary was connected to a high voltage DC
source and the base on which the substrate was placed under Electrohydrodynamics atomization process consists of spraying
the metallic capillary was connected to ground. The DC signal functional ink through capillary under the effects of electric eld.
was generated by a function generator (Hewlett Packard 33120A) When a functional ink was passed through a capillary at a ow
and this signal was amplied using high power DC amplier (TREK rate, in the absence of any electric eld drops of ink larger than
Model 610E). An oscilloscope (Hewlett Packard 54602B 150 MHz) the capillary diameter were formed and dropped on substrate.
was attached to monitor the voltage. A high speed CCD camera The voltage was increased gradually, keeping the standoff distance
328 M. Zubair et al. / Chemical Engineering Journal 253 (2014) 325331

at 10 mm and the ow rate of 100 ll/h. The size of drops falling

down on the substrate decrease with the increase of electric eld.
The stage when smaller droplets start detaching from meniscus is
known as the micro dripping which was observed at the voltage of
2.2 kV. Increase of voltage to 2.4 kV brought the meniscus in unsta-
ble cone jet. Here cone jet oscillated and ejected smaller droplet.
Further increase in voltage to 2.8 kV brought the stable cone jet
mode, which was used to spray. Further increase in voltage
brought the meniscus in multi-jet mode at the voltage of 3.0 kV.
Different modes of electrohydrodynamics phenomena are shown
in Fig. 3. As the ow rate affects the potential difference required
for the creation of stable cone jet mode [35], so an operating enve-
lope was explored. At a certain ow rate, the voltage was increased
to observe the different modes of EHDA phenomena. The values of
voltage for corresponding EHDA modes were recoded. The operat-
ing envelope was plotted by repeating the experiment with differ-
ent ow rates [36,37]. The operating envelope of CdSe/ZnS
quantum dots is shown in Fig. 4.
The surface morphology of thin layers of the fabricated
Fig. 4. Working Envelop of CdSe/ZnS Quantum Dots at different ow rates.
PEDOT:PSS and MEH-PPV onto ITO substrate were analyzed. The
FE-SEM images of thin lms of PEDOT:PSS and MEH-PPV are
shown in Fig. 5. The coated layers were non-porous, homogenous, cathode and was connected to the negative terminal of probe sta-
and densely packed. No defects like crakes or craters were tion. The energies of materials dene the movements of holes and
observed in thin lms. QDs were sprayed using EHDA technique electrons. The H-LED device energy diagram is shown in Fig. 8. The
on PEDOT:PSS layer. Structural integrity of QDs was investigated highest occupied molecular orbital (HOMO), lowest unoccupied
by TEM analysis. The TEM image of QDs is shown in Fig. 6 where molecular orbitals (LUMO) of ITO [40], PEDOT:PSS [41] and MEH-
inset shows the lattice spacing of 0.4 nm. The average particle size PPV [42] were taken from the literature while the HOMO & LUMO
of QDs was about 6.58 nm. values of QDs were measured by cyclic voltammetry. The HOMO
To nd the optimized thickness to of the emissive layer for H- and LUMO of QDs were found out to be 5.785 eV and
LED device application, the standoff distance was varied form 3.555 eV respectively with energy band gap of 2.23 eV. The PED-
10 mm to 5 mm. With the decrease of standoff distance, a decrease OT:PSS with high work function of 5.1 eV transports the holes
in the spray area was observed; hence, the thickness of the into QDs layer, where HOMO of QDs is 5.785 eV. The electrons
emissive layer was increased. The layer thickness change with from the low work function of aluminum move into MEH-PPV,
respect to change in standoff distance is presented in Table 1. which transport the electrons into the QDs. In the QDs layer the
The normalized photoluminance intensity (PL) of QDs solution holes combine with electrons to emit photons.
and absorbance spectrum of QDs layer is shown in Fig. 7. The The current density with respect to voltage of H-LED devices on
QDs showed a single narrow peak at 634 nm. In visible light glass substrates at different standoff distances and PET substrate at
spectrum, this wavelength lies in red color region. The absorbance 6 mm standoff distance are shown in Fig. 9. Here it can be seen that
spectrum of CdSe/ZnS QDs layer corresponds to the reported hybrid device (ITO/PEDOT:PSS/QDs/MEH-PPV/Al) shows non-ideal,
values in literature [38,39]. schottky diode behavior with hopping charge transport mecha-
The electrical characterization of H-LED device was performed nism [43,44]. The current density of H-LED increased with the
to nd the performance of the device (ITO/PEDOT:PSS/QDs/MEH- decrease of standoff distance. The decrease of standoff distance
PPV/Al). The ITO acted as anode and was connected to positive increased the lm thickness as area of spray was reduced. At the
terminal of probe station while the aluminum was used as the standoff distance of 6 mm, highest current density was achieved

Fig. 3. EHDA phenomena where (a) shows the metallic capillary, (b) dripping mode, (c) micro-dripping mode, (d) unstable cone jet mode, (e) stable cone jet mode, (f) multi
jet cone mode.
M. Zubair et al. / Chemical Engineering Journal 253 (2014) 325331 329

Fig. 5. FE-SEM images of (a) PEDOT:PSS and (b) MEH-PPV thin layers.

Fig. 7. Photoluminescence and absorbance spectrum of CdSe/ZnS Quantum dots

with inset showing quantum dots ink.

Fig. 6. TEM image of CdSe/ZnS quantum dots showing the size of QDs around 6.5
8 nm.

Table 1
Thickness of thin layer of QDs at different standoff distance.

Standoff Distance (mm) Thickness of CdSe/ZnS QDs layer (nm)

10 183
9 225
8 262
6 350
5 1156

but further decreasing the standoff distance to 5 mm, wetting in

electrohydrodynamics atomization observed. In wetting phenom- Fig. 8. Energy Level Diagram of H-LED device.
ena, wet lm on substrate was observed instead of a semi-dry lm
after performing EHDA as droplet falls on substrate before they are
properly atomized into micron-sized particles. This wetting caused of bending as shown in Fig. 10. The organic layers did not show
the thin layer thickness to jump from 350 nm to 1156 nm and any degradation while lower current densities were attributed to
hence a thick layer of QDs by wetting was achieved which showed the brittle nature of ITO [45]. The recorded electroluminance of
reduced current. hybrid device on glass and PET substrate with optimized distance
The exible device was xed in a lab made motorized cyclic are shown in Fig. 11. The recorded emission or electroluminance
bending xture by which the device was tested at 5 mm radius intensity of QDs H-LEDs was found at optimized distance was
of curvature. The IV measurement was performed after number the same wavelength as shown in the photoluminescence
330 M. Zubair et al. / Chemical Engineering Journal 253 (2014) 325331

Fig. 9. Log(I) V curves of hybrid devices with QD sprayed at different standoff

distances on glass and PET substrates with inset showing IV characterization. Fig. 12. Luminance of the hybrid CdSe/ZnS QD device with respect to voltage is
shown on PET and glass substrate. The inset shows the H-LED at on-state.

Fig. 10. IV curves of exible H-LED after cyclic bending testing.

Fig. 13. Color coordinates on CIE chromaticity chart of H-LED at different voltages
on PET substrate are shown by black square while white cross represents the H-LED
devices on glass substrate.

spectrum of QDs ink. This electroluminance intensity at the wave-

length 634 nm showed that the achieved luminescence of the
device was by QDs layer and MEH-PPV acted as electron transport
layer and was not involved in any emission of light. The variation
luminance of H-LED with optimized 6 mm standoff distance with
voltage is shown in Fig. 12. The inset of the Fig. 12 shows the
glowing H-LED at on state on exible substrate. Maximum
luminescence of 2.4 lux was obtained at 15 V. The wavelength of
emission was at 634 nm, which lies in pure red region of visible
color range. The Commission International dEclairage (CIE) coordi-
nates (x, y) were also obtained by lux meter are shown in Fig. 13 on
CIE chromaticity chart with black squares show the H-LED on PET
Fig. 11. Electroluminescence of CdSe/ZnS quantum dots H-LED on glass and exible substrate while white cross represent the H-LED on glass
substrate. substrates at different voltages.
M. Zubair et al. / Chemical Engineering Journal 253 (2014) 325331 331

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