www.MaterialsViews.
com
Direct Printing of Reduced Graphene Oxide on Planar
or Highly Curved Surfaces with High Resolutions Using
Electrohydrodynamics
Byeong Wan An, Kukjoo Kim, Mijung Kim, So-Yun Kim, Seung-Hyun Hur,*
and Jang-Ung Park*
Graphene, a carbon monatomic layer with a sp2-bonded
honeycomb structure, has been recently investigated as a
promising 2D material thanks to its unique material prop-
erties of high carrier mobility,[1–3] mechanical flexibility,[1,4]
thermal conductivity,[5] and optical transparency.[6] Although
graphene exfoliated from graphite mechanically[2] still gives
the best properties with high purity and low defects, this exfo-
liation process has limitation about large-scale production.
Thus, formation of graphene in large area is necessary for
widespread applications in electronics, including touch screen
panels,[7] sensors,[8] light-emitting diodes,[9] supercapacitors,[10]
and solar cells.[11,12] Scalable graphene synthesis methods, such
as chemical vapor deposition (CVD) on catalytic surfaces and
epitaxial growth on SiC, can synthesize graphene uniformly
in large areas. However, these methods still use conventional
multiple steps of lithography and dry etching for patterning,
and the lithography process does not facilitate patterning
on nonplanar substrates. Besides, the CVD method mostly
requires additional processes for transferring the graphene
layer from the catalyst surfaces to other target substrates.
Instead, another promising alternative method is liquid
phase exfoliation (LPE).[13–16] Suspensions of graphene
oxides (GOs) can be obtained by the oxidation of graphite
using several processes proposed by Brodie, Staudenmeier,
and Hummers. Due to the easiness and controllability of
the reaction, the Hummers methods are more generally
used over others in the recent studies. After the oxidation,
large amounts of oxygen-related functional groups, such
as hydroxyl or epoxide groups, are introduced to the basal
B. W. An, Dr. K. Kim, M. Kim, S.-Y. Kim, Prof. J.-U. Park
School of Materials Science and Engineering
School of Energy and Chemical Engineering
Low-Dimensional Carbon Materials Center
Ulsan National Institute of Science
and Technology (UNIST)
Ulsan 689-789, Republic of Korea
E-mail: jangung@unist.ac.kr
Prof. S.-H. Hur
School of Chemical Engineering and Bioengineering
University of Ulsan
Daehak-ro 102, Nam-gu, Ulsan 680-749, Republic of Korea
E-mail: shhur@ulsan.ac.kr
DOI: 10.1002/smll.201403131
small 2015, 11, No. 19, 2263–2268 © 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Printed Electronics
plane and carboxyl or carbonyl groups to the edges of indi-
vidual GO sheet, which make the GO hydrophilic and well
dispersed to many polar solvents such as water, dimethyl
sulfoxide (DMSO), N,N′-dimethylformamide (DMF). The
electrically conductive reduced graphene oxide (RGO) can
be produced from the insulating GO by chemical or thermal
reduction through the recovery of sp2-bonds. Chemical
reduction using hydrazine or phenylhydrazine in the pres-
ence of DMF and water is one of the easiest methods to con-
vert GO to RGO in the laboratory, due to their effectiveness
and fast reaction. Solvothermal reduction with N-methyl-
2-pyrrolidone (NMP) is also considered as a useful method
because toxic chemicals can be avoided during the reaction.
There remains some amount of functional groups even after
chemical and solvothermal reduction, which enables RGO
to be well dispersible to various kinds of solvents. Moreover,
by controlling the amount of remaining functional groups or
introducing other functionality to RGO, its electrical proper-
ties and solubility can be easily controlled to be adjusted to
the main fabrication and target applications.
The suspensions of RGO can be used as inks, and printing
techniques enable the suspensions to be printed directly onto
target substrates with the desired patterns. Patterning of gra-
phene has been achieved using various methods including
mask-assisted plasma etching[17–19] or growth on prepatterned
catalyst films,[6,20] which requires costly multiple steps with
limited scalability. Compared to those conventional patterning
process, direct printing,[21–24] or laser direct writing[25–28]
approaches are relatively simple and offer low-cost, large-area
fabrications of devices. (See Table S1, Supporting Informa-
tion.) Among diverse printing methods, inkjet technique is
of interest due to desirable features including (1) the capa-
bility of fabricating arbitrary pattern designs, where changes
can be achieved readily through software, (2) the reduction
in material waste by depositing functional inks only where
they are required,[29] and (3) compatibility with large-area
substrates.[30–32] Growing numbers of reports describe inkjet
printing of graphene using commercially available inkjet
systems with demonstrations on fabrications of devices or
device components such as flexible electrodes,[21,33,34] radio
frequency identification (RFID) antennas,[22] display[35] and
organic transistors.[23,24] Conventional inkjet printers gen-
erate ejection of droplets from nozzle orifices with the aid
of thermal or acoustic force.[36] However, the finest feature
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www.MaterialsViews.com

size that can be reliably achieved by con-

ventional inkjet printer, or simply the
resolution, is ≈20–30 µm,[34,37–39] which is
too large for many potential applications.
As nozzle sizes reduce in order to eject
smaller droplets for higher printing resolu-
tion, the required magnitude of the pres-
sure induced by the printheads increases
beyond the elevated viscous forces and
surface tension that interrupt droplet ejec-
tion. Difficulties in reducing the fluid resist-
ance and increasing the pressure inside the Figure 1. High-resolution printing of RGO. a) Schematic image of e-jet system. b) An optical
nozzle indicate obstacles against improving image (scale bar, 50 µm) and c) AFM image of a line printed using a 5-µm-inner-diameter
the resolution of thermal or piezoelectric nozzle and RGO ink with line-width of 5 µm. Thickness of ≈8 nm was achieved by printing
inkjet printheads.[40] Furthermore, sus- 15 times. d) Raman spectrum of the printed and spin-coated RGO ink.
pensions of large particles like GOs also
restrict the nozzle size reduction owing to the nozzle clog- Figure 1a shows schematic image of the e-jet printing
ging.[34] Thus, direct printing of graphene patterns with high system. For the nozzle fabrication, Cr (10 nm), Cu (100 nm),
resolutions using inkjet remains a challenging topic. and Au (10 nm) layers were successively deposited to the out-
Here, we report direct, electrohydrodynamic inkjet (e-jet) side of glass capillaries with inner diameters of 5 µm. Then tip
printing of RGO for high-resolution patterns. e-jet utilizes areas of these pipettes were dipped into 1H,1H,2H,2H-per-
electric fields, instead of thermal or acoustic force, to induce fluorodecanthiol solution (0.01 wt% in DMF) for 30 min to
ejection of the jet or droplets toward a substrate. An applied form hydrophobic self-assembled layer on the surface of the
electric field to the nozzle can generate a fine liquid jet at metal-coated nozzle. After connecting this metal-coated nozzle
the tip of a conical ink meniscus with the aid of the electro- to an ink reservoir, the suspension of RGO was delivered as an
static force. Because this jet diameter is much thinner than the ink from the reservoir to the nozzle tip by a pneumatic pres-
nozzle size, e-jet printing is advantageous to control the flow sure regulator to form a pendent ink meniscus. Silicon wafers
rate precisely and hence to achieve higher resolution. To our with 300 nm-thick SiO2 top layers were used as substrates, and
knowledge, its potential to fabricate high-resolution (<≈10 µm they were exposed by a UVO cleaner (AH1700, AHTECH
in line-width) patterns of RGO has not been examined, as a LTS) for 30 min before printing. The wafer was located on a
direct printing method. In this paper, we directly printed sus- conductive plate, which was mounted on a moving stage, with
pensions of RGO using this e-jet technique, and successfully a separation of ≈100 µm to the nozzle.[28,41] DC bias voltage
formed complex geometries of electrically conductive patterns, was applied between the plate and the prepared nozzle for
including alphabetic letters, with high resolutions (line width: printing. This applied electric field led to the accumulation of
≈5 µm). Flat substrates and even on highly curved surfaces (the mobile ions to the surface of the ink and, in turn, induced the
radius of curvature: ≈50–65 µm) can be used for this high-reso- deformation of the meniscus to a cone shape, which is known
lution printing of RGO. Recognition of counterfeit coins using as a Taylor cone, and finally brought the ejections of a thin
fine patterns of RGO, and fabrication of all-printed transistors liquid jet from the tip of the cone onto the substrate. This ejec-
demonstrate potential applications in security and electronics. tion reduced the amount of charge from the ink at the nozzle
Suspensions of GO were produced by the oxidation of tip, and led to the retrieval of the meniscus back to hemispher-
expanded graphite (Grade 1721-Asbury Carbon) via the ical shape. Optimizing the applied voltage and the stage trans-
modified Hummers method using KMnO4 and sulfuric acid, lations enabled desirable operation of the e-jet system. After
as reported previously. Initially, 1 mL of hydrazine diluted in completing the printing step, the printed sample was dried at
5 mL of deionized water (DI water) was added to 10 mL of 250 °C for 30 min for solvent evaporation. Figure 1b,c shows
aqueous GO solution (10 mg mL−1) with subsequent ultra- an optical microscopic image and atomic force microscopy
sonication for 4 min to make homogeneous solution. Then, (AFM) image of a line printed using the RGO suspension
the solution was kept at 90 °C for 2 h with magnetic stirring to at a substrate translation speed of 0.05 mm s−1 with 15 times
convert GO to RGO. The RGO was washed with copious DI of printing repetitions. Multiple-pass printing was used to
water and redispersed in DMF (1 mg mL−1). Addition of eth- increase the thickness of the printed patterns due to limitation
ylene glycol (30 wt%) to the RGO suspension for retarding on increasing ink concentration, and a continuous line pattern
the nozzle clogging completes synthesis of the RGO ink. The with width of 5 µm and thickness of ≈8 nm was obtained, as
reduction degree of the RGO in the prepared ink was charac- shown in Figure 1b,c. These results represent a higher resolu-
terized by elemental analysis (EA) and x-ray photoelectron tion compared to conventional thermal or piezoelectric inkjet
spectroscopy (XPS). (See the Supporting Information.) XPS printing of graphene. As shown in Figure 1d, the e-jet printed
spectra for GO and RGO in Figure S1, Supporting Infor- RGO exhibits similar Raman spectrum, compared to the spin-
mation, indicate highly reduced oxygen-related functional coated RGO film, which indicates that the e-jet printing pro-
groups after reduction. The EA analysis of GO and RGO cess induces negligible damage on the RGO flakes.
also shows increased C/O ratio from 1.09% to 5.35% after Figure 2a shows an optical image of alphabetic patterns
reduction, as listed in Table S2, Supporting Information. with gradient colors by controlling the pattern thickness

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www.MaterialsViews.com

Figure 2. Thickness control of the printed patterns. a) An optical image of alphabetic patterns with gradient colors by controlling thickness (line
width: about 4–5 µm). A 5-µm-inner-diameter nozzle was used, and the thickness of the pattern was adjusted by changing printing times locally.
(Scale bar, 200 µm). b) AFM depth profiles of portions of the alphabet patterns in Figure 2a). c) Thickness of the printed RGO patterns in terms
of printing times. d) Linear change in the resistance of the RGO line (width: ≈5 µm, thickness: ≈40 nm) with length. Resistivity is ≈0.0013 Ω m.

(line width: about 4–5 µm). A 5-µm-inner-diameter nozzle
was used, and the thickness of the pattern was controlled by
adjusting printing repetitions locally. For example, Figure 2b
shows AFM depth profiles of local portions of the “GRA-
PHENE” alphabet patterns. The use of this fine nozzle can
produce small volumes of the ejected droplets in subpicoliter
ranges and therefore can significantly fasten drying process
of the droplets on substrates with minimizing dewetting[42] or
coffee ring[43] effect. The pattern thickness increases linearly
with printing repetitions (Figure 2c), which induces different
colors of the patterns shown in Figure 2a. Also, the printed
RGO line exhibits linear increase of electric resistance with
the length of this line (Figure 2d). This printed RGO pattern
shows resistivity of 0.0013 Ω m.
The resolution of the printed patterns can be controlled
by modulating the nozzle diameter. As shown in Figure 3a,
for example, an alphabetic pattern “e” was printed with
10 µm in line-width on a thermally grown SiO2 (300 nm)/Si
wafer, using a 10-µm-inner-diameter nozzle. Instead of the
planar surfaces of wafers, nonplanar surfaces can also be used
for e-jet printing. For this printing on nonplanar substrates,
the height between the nozzle and substrate should be main-
tained constantly during printing process, because the mag-
nitude of the electric field at the edge of the nozzle tip can
determine the overall flow rate and printing resolutions in
electrohydrodynamics.[28,41,44] In our e-jet setup, a computer-
controlled translation stage with x, y, and z axes along with
a biaxial tilting stage offers adjustments to assure a precise
movement in xy-plane while maintaining the height during
the printing process on nonplanar substrates. Figure 3b pre-
sents the e-jet printed RGO alphabetic patterns (line width:
≈5 µm) on the highly curved surface of a microcapillary with
the radius of curvature in the range between 50 and 65 µm.
Counterfeit coin recognition for security indicates an
important application field that can utilize this high-resolu-
tion printing capability of RGO on planar or nonplanar sur-
faces. For this purpose, a fine alphabetic pattern, G, was e-jet
printed using the RGO ink on the recessed, rough surface of
a metal coin which is composed of Cu–Zn–Ni alloy (center)
and cupronickel (edge). The high transmittance of RGO ena-
bles this printed pattern to be indistinctive with the naked
eye, as shown in Figure 3c. Here, the printed RGO layer
can act as a protection layer against oxidation of the coin.
Carbon allotropes with the sp2 hybridized orbital make a dif-
fusion barrier acting as a physical separation layer between
oxygen molecules and metal surfaces. Also, high thermal and
chemical resistivity of graphene is advantageous for its use
as the protection layer against oxidation.[45–47] When this coin
was thermally oxidized by heating it at 200 °C on a hotplate,
the printed RGO pattern prevented the oxidation of the coin
locally, and hence color of the printed area became visible
distinguishably (Figure 3d). Reduction of the oxidized coin
enabled the RGO pattern to be almost indistinctive again.
As a demonstration of all-printed transistor fabrication
with no use of photolithography process, electrodes of source/
drain and the RGO channel were formed using e-jet on a ther-
mally grown SiO2 (300 nm)/Si wafer. This approach to adapt
high-resolution printing technique is significant for cost-
effective next-generation electronics. The fabrication pro-
cess began with depositing uniform metal layers of Cr (5 nm,
adhesive layer) and Au (100 nm, main conducting layer) onto
the wafer. As illustrated in Figure 4a, photocurable poly-
urethane (NOA74, Norland Optical Adhesives, Inc.) was e-jet
printed and cured as an etch-resist using a nozzle with 1 µm
inner diameter. Then wet etching of the uncovered area of
deposited metal defined source/drain electrodes with printing
resolution of 2 ± 0.4 µm in line-width. After removing the
polyurethane resist using oxygen plasma (20 sccm of oxygen
gas flow, chamber pressure of 250 mTorr, 150 W, 5 min), the
RGO printing using e-jet formed the channel part and com-
pleted the device fabrication. Figure 4b,c shows optical micro-
scopic images and an AFM image of the printed transistor
with channel length of ≈3 µm. Drain current (ID) versus gate
bias (VG) of the transistor was analyzed in ambient condition

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 communications
Figure 3. High-resolution printing on nonplanar surfaces. a) Optical
image of an alphabetic pattern with the line width of 10 µm.
A 10-µm-inner-diameter nozzle was used. (Scale bar, 50 µm).
b) SEM images of the RGO patterns printed on the sidewall of a glass
microcapillary as a substrate, using the 5-µm-inner-diameter nozzle
(line width: ≈5 µm). The microcapillary has a cone geometry as shown
in the top inset, and radius of the substrate is in the range between
50 and 65 µm. The white scale bars are 100 µm. c) Photo (left) and
optical image (right) of a coin composed of Cu–Zn–Ni alloy (center) and
cupronickel (edge), where an alphabet pattern “G” was printed before
oxidation. The black scale bar is 1 cm and white scale bar is 50 µm.
d) The printed coin after oxidation (200 °C for 20 min on a hotplate).
Although the printed area was barely visible before oxidation, the
printed RGO acts as a passivation layer against oxidation and the
printed pattern becomes distinguishably visible. The black scale bar is
1 cm and white scale bar is 50 µm.
at room temperature (Figure 4d). The transfer curve shows
ambipolar characteristics that coincide with the previously
reported semimetallic characteristics of RGO,[48,49] with a
charge neutrality point close to ≈0 V. This transistor showed
mobility of ≈6 cm2 V−1 s−1, estimated using a common metal–
oxide–semiconductor thin film transistor model.
In conclusion, we demonstrate here the ability to print, in
a controlled fashion, high-resolution patterns of RGO, by use
of the electrohydrodynamic inkjet. Large-scale patterns of
RGO with complex geometries and feature sizes in ≈5 µm of
line-width can be printed readily, suitable for use in various
applications in security and electronics. Also, direct printing
capability of RGO on both flat and highly curved surfaces
described here offers unique potential for 3D, integrated
devices using printed electronics in the future.
2266 www.small-journal.com © 2015 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.MaterialsViews.com
Experimental Section
Preparation of Nozzles: Cr (10 nm), Cu (100 nm), and Au
(10 nm) layers were deposited to glass capillaries with various inner
diameters (0.5–30 µm) using a thermal evaporation system. The
metal-coated nozzle was dipped into 1H,1H,2H,2H-perfluorode-
canethiol (Sigma-Aldrich) solution (0.1 wt% in DMF) for 30 min to
form hydrophobic layer on the metal-coated nozzle surface to pre-
vent nozzle wetting phenomena. A pneumatic pressure pump was
connected to the nozzle to help the inks to reach the nozzle tip.
Preparation of RGO Inks: The GO suspension was prepared by
the oxidation of expanded graphite (Grade 1721-Asbury Carbon)
via the modified Hummers method using KMnO4 and sulfuric acid.
Initially, 1 mL of hydrazine diluted in 5 mL of DI water was added
to 10 mL of aqueous GO solution (10 mg mL−1) with subsequent
ultrasonication for 4 min to make homogeneous solution. Then,
the solution was kept at 90 °C for 2 h with magnetic stirring to con-
vert GO to RGO. The RGO was washed with copious DI water and
redispersed in DMF (1 mg mL−1) to form the ink solution.
Preparation of Substrates: Thermally grown SiO2 (300 nm)/Si
wafers were used as substrates. Cr (5 nm) and Au (100 nm) layers
were coated onto SiO2/Si. The wafer was electrically grounded
during printing.
Transistor Fabrications: On the Cr/Au-deposited SiO2/Si sub-
strate, a UV-curable polyurethane etching resist layer (NOA74,
Norland Optical Adhesives, Inc.) with the minimum line width
of 2 ± 0.4 µm was printed using the e-jet system and a nozzle
with 1-µm-inner-diameter. The e-jet printed resist was cured
by exposing UV light (≈1 J cm−2). The Cr/Au layer was pat-
terned using wet etching process (Au etchant: trifluoroacetic
acid, Transen, Cr etchant: Cr mask etchant, Transen). And the
resist was removed by O2 plasma etching (reactive ion etching,
20 sccm oxygen gas flow, chamber pressure of 250 mTorr, 150 W,
5 min). Then the RGO ink was e-jet printed onto the source/drain
pattern as a channel material. The RGO ink was printed using a
5-µm-inner-diameter nozzle and 10-µm-inner-diameter nozzle
for controlling the resolutions. Remaining organic solvents were
removed by annealing the printed RGO patterns at 250 °C for
30 min.
Electrical Characterization: Electrical characterizations were
conducted with the transfer and output characteristic meas-
urement using a semiconductor parametric analyzer (Keithley
4200-SCS).
Supporting Information
Supporting Information is available from the Wiley Online Library
or from the author.
Acknowledgements
B.W.A. and K.K. contributed equally to this work. This work was
supported by Agency for Defense Development as a collaborative
preliminary core technology research project.
small 2015, 11, No. 19, 2263–2268
www.MaterialsViews.com

Figure 4. All-printed field-effect transistor (FET). a) Schematic diagram of the printing procedures. First, a UV-curable polyurethane etch-resist
(NOA74, Norland Optical Adhesives, Inc.) was printed on the Au surfaces for source/drain patterns using a 1-µm-inner-diameter nozzle. After wet
etching and removing the printed resist, source/drain patterns were formed. Then the RGO ink was printed for the local channel area of FET. In
this way, bottom-gate FETs can be printed without use of photolithography. b) Optical images of the all-printed RGO FETs. Bottom image shows a
magnified view of the channel regime (length: 3 µm, width: 70 µm). The upper scale bar is 200 µm and bottom (scale bar, 30 µm). c) AFM image
of the printed channel area. d) Transfer curve of the all-printed FET. (Hole mobility: ≈6 cm2 V−1 s, Vd: 10 V).

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