Phys. Status Solidi A 213, No. 6, 1403–1409 (2016) / DOI 10.1002/pssa.

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Part of Topical Section on
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applications and materials science

A study on the thermal sintering

process of silver nanoparticle inkjet inks
to achieve smooth and highly
conducting silver layers
Glen Vandevenne1,2, Wouter Marchal1,2, Inge Verboven1,2, Jeroen Drijkoningen1,3, Jan D’Haen1,2,
Marlies K. Van Bael1,2, An Hardy1,2, and Wim Deferme*,1,3
1
Institute for Materials Research (IMO), Hasselt University, Wetenschapspark 1, 3590 Diepenbeek, Belgium
2
IMEC vzw – Division IMOMEC, Wetenschapspark 1, 3590 Diepenbeek, Belgium
3
Flanders Make vzw, Oude Diestersebaan 133, 3920 Lommel, Belgium

Received 23 November 2015, revised 30 January 2016, accepted 19 February 2016

Published online 11 March 2016

Keywords inkjet printing, nanoparticles, silver, thermal sintering, thin films

* Corresponding author: e-mail wim.deferme@uhasselt.be, Phone: þ32(0) 11 26 88 74, Fax: þ32(0)11 268899

Silver nanoparticle inkjet inks are commonly used to print
electrically conductive patterns, such as sensors or electrodes
in organic light emitting diodes (OLEDs) or organic
photovoltaic devices (OPVs). After printing, a sintering step
is required to transform the printed layer into an electrically
conductive one. Gaining more insight into the occurring
phenomena during this post-treatment step is necessary when
applying different kinds of inkjet ink. Therefore, in this work
the commercially available silver nanoparticle inkjet ink
Metalon JS-B30G from Novacentrix is characterised during
the different stages in the printing and thermal sintering
sequence. The pre-printing and post-sintering characterisation
proves that the inkjet ink used has got the right material
parameters, such as viscosity and particle size. Silver layers
with sheet resistances of 40 mV/sq were obtained with an
average roughness lower than 10 nm. The experiments
performed show the different stages during the thermal
sintering procedure. Based on this, suitable thermal sintering
parameters are defined leading to application of these
conductive silver layers in OLEDs.

ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

1 Introduction Inkjet printing is a printing method
that traces its roots back to the beginning of the 19th century.
Ever since, this technique has found its applications mainly
in the publishing and graphic industries, especially for short
series or customised packaging. [1, 2] During the 1960s, dr.
Sweet developed the first Continuous InkJet (CIJ) printer
[1, 3]. This type of printer jets droplets continuously. The
droplets that are not intended to reach the substrate, get
charged and are subsequently deflected into a recycling
system that guides them back to the ink reservoir. Another
approach is drop-on-demand (DOD) inkjet printing. One of
the first DOD systems was built by the Radio Corporation of
America [1]. Here, a droplet is only jetted when it is required
to. This way of printing eliminates the need for a charging
(deflection) and a recycling mechanism and is therefore
more interesting to deposit functional materials, since those
inks will no longer be exposed to an electric field. Moreover,
the functional materials will be exposed only once to
ambient conditions (instead of potentially multiple times
with the CIJ), so subsequent degradation can be avoided.
Within the DOD printers, different print head types can be
distinguished. A first one is the thermal inkjet print head,
which is typically used for office applications. Those print
heads contain a resistor that is heated up when a droplet
needs to be jetted. The heat causes the creation of a vapour
bubble that pushes a small amount of ink through the nozzle
orifice. At that moment, the current to the heating resistor is
switched off, causing a heat flux stop and therefore the
collapse of the vapour bubble. Due to this collapse, a
negative pressure is created inside the print head, resulting
in a pushback of the ink and a break-off of the ink droplet
outside the print head. To avoid thermal damage to the

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functional ink, another actuator type can be chosen, e.g., a
piezo-electrical one. The piezo elements in the print heads
deform by an applied voltage signal. Depending on the
shape of this signal, an either positive or negative pressure is
created in the print head causing droplets to jet. The first
demonstration of a high-resolution DOD print head was
performed by Sirringhaus et al. [4]. Nowadays, structures
with dimensions as small as 14–25 mm can be deposited
without surface treatment [5], which is comparable to the
smallest features reached in the semiconductor industry of
the 1970s. Via the use of surface treatments, feature sizes of
5 mm have been attained [1]. This contactless direct writing
method is used for several applications: e.g., printed circuit
board (PCB) manufacturing [6, 7], radio frequency
identification (RFID) tags [8–10], solar cells [11–13],
organic light emitting devices (OLEDs) [14–16], energy
storage devices [17], displays [18, 19], sensors [1, 29], etc.
For every new application, a new inkjet ink has to be
developed. Electrically conductive inkjet inks can be
categorised into three groups: suspensions of nanoparticles,
organometallic compounds in solution and conductive
polymers [20]. This work mainly focuses upon the first
group of inks based on silver nanoparticles. One of the major
ingredients here is the solvent (blend), which must easily
evaporate after depositing [1]. Nonetheless, evaporation
must not happen too fast in order to avoid nozzle clogging
due to dried ink at the orifice. Apart from the evaporation
rate, the solvent (blend) must have a well-tuned dynamic
viscosity in order to obtain a controlled jetting behaviour
and a right surface tension to be able to overcome the surface
tension at the meniscus. The silver nanoparticles, as the
main ingredient, are covered with a capping polymer to
prevent clustering of the nanoparticles in the ink car-
tridge [21]. To transform the printed layer into a conductive
one, a sintering procedure is required, as shown in Fig. 1.
First, the solvent (blend) must be evaporated. As a second
step, the polymer capping shell needs to be removed from
the silver nanoparticles, after which the real sintering of the
particles can occur. Since the particle size is in the range of
nanometres, the sintering temperature can be much lower
than in the case of bulk material [22]. Still a temperature
around 200 8C is required for 30 min for inks consisting out
of nanoparticles and thermally sintered in ambient
conditions [32].
The polymer polyvinylpyrrolidone (PVP) is commonly
used as a capping agent [23] and has a glass transition
temperature of about 180 8C, depending slightly on the
molecular weight [24]. This explains why a temperature of
at least 180 8C or even more is needed to reach a sintered
Figure 1 Sintering procedure of Ag nanoparticle inkjet inks [21].
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
layer, since sintering of the silver nanoparticles is
impossible when they are still capped. Therefore, printing
and sintering on heat-sensitive substrates or devices is not
possible via printing and thermal sintering of capped
nanoparticles.
In this work, the printing characteristics of the
commercially available silver nanoparticle ink JS-B30G
from Novacentrix are evaluated before printing. More
insight in the materials’ behaviour during the sintering
procedure itself is obtained via thermogravimetric and
differential thermal analysis (TGA-DTA) and atomic force
microscopy (AFM) measurements. This is expected to result
in silver layers with the optimal morphological and
electrical properties. The optimal sintering temperature
and time is researched by means of subsequent experiments,
after which the sintered silver layer is subjected to electrical
and morphological characterisation. As a last step, the
inkjet-printed silver patterns are used as electrodes for
OLEDs to show their applicability in state-of-the-art
applications.
2 Materials and methods Commercially available
Metalon nanoparticle silver JS-B30G ink is inkjet printed
upon glass substrates. Those are cleaned ultrasonically in
acetone during 30 min at room temperature and afterwards
dried with a nitrogen gun.
Before printing, the ink is characterised by transmis-
sion electron microscopy (TEM) on a Tecnai Spirit Fei
setup. Viscosity measurements are performed on an AR-
G2 rheometer of TA-Instruments and an SDT Q600
device of TA-Instruments is used for the TGA-DTA
analysis.
A Fujifilm Dimatix DMP 2800 series drop-on-demand
(DOD) inkjet printer operates during the printing experi-
ments with 10 pl cartridges. The printed samples were
thermally treated in a box oven under ambient conditions.
As a post-sintering characterisation, the sheet resistance
of the silver layers is measured by a home-built van der
Pauw measurement system. Information on the topology of
the printed layers is obtained via profilometry measurements
(Dektak XT from Bruker) and AFM measurements
(Multimode 8 from Bruker).
OLEDs are produced upon ITO-coated glass substrates
bought from Visiotek Systems.
3 Results and discussion
3.1 Transmission electron microscopy (TEM)
Before printing, the size of the silver nanoparticles is
checked in order to avoid nozzle clogging due to an
oversized particle in comparison to nozzle size ratio. The
sides of the square-shaped nozzles of the Dimatix cartridges
used, are measured to be 21 mm. Particles with a size larger
than 5% of the orifice diameter (in this case 1 mm) may
cause nozzle clogging according to the print head
supplier [30]. In literature, a stricter rule of thumb is
used: the particle size must not exceed 1% of the orifice
diameter [1].
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Phys. Status Solidi A 213, No. 6 (2016) 1405

Moreover, this ink presents a Newtonian behaviour whereas

most of the commercial available inks are non-
Newtonian [25]. This means that the ink’s shear stress
scales linearly with the shear rate. Therefore, the behaviour
of the ink remains unaffected at various printing frequencies
without adapting the jetting waveform or other printing
parameters.

3.3 Printing experiments To characterise the print-

ing properties of the ink, 10 by 10 mm squares were printed
on ultrasonically cleaned glass substrates. A toatl of 10 pl
droplets are printed with a drop spacing of 10 and 15 mm.
First, the focus is directed to the sintering procedure after
printing. In order to understand the occurring phenomena, a
TGA-DTA measurement is performed on the inkjet ink to
investigate both mass change and heat flow as a function of
temperature (Fig. 3). Subsequently, a thermal sintering
procedure is performed on a printed layer, using the same
heating conditions as in the TGA-DTA, to map the changes
in resistivity and morphology during the sintering proce-
Figure 2 TEM picture showing the silver nanoparticles in JS-
dure. As a second series of experiments, the thermal
B30G ink. Particle sizes ranging from 10 to 40 nm can be observed.
sintering procedure is further optimised. Inkjet-printed
structures with different drop spacings are thermally
TEM measurements show particle sizes ranging from 10
sintered at a fixed temperature for various durations. The
to 40 nm meeting the rule of thumb of 1% of the orifice
sheet resistance and the roughness of these samples
diameter, i.e., 200 nm, as is shown in Fig. 2.
are investigated. Once the optimal sintering conditions
have been found, the inkjet-printed silver layers and
3.2 Viscosity measurements Beside the nanoparti-
structures are implemented into different applications.
cle size, an additional important material parameter to be
taken into account, is the dynamic viscosity, which must be
3.4 Thermal analysis DTA measurements are pre-
between 1 and 25 cP [1]. According to the manufacturer of
sented in Fig. 3. Before the start of the measurement, the ink
the inkjet printer, the ink applied needs to have a dynamic
is heated up to 80 8C to remove the major part of the solvent
viscosity between 10 and 12 cP at operation temperature
(blend) and subsequently measure the decrease in mass
[31]. Viscosity measurements performed at ambient
more precisely. Afterwards, the residue is cooled down,
conditions have proven that JS-B30G ink has a viscosity
after which the DTA measurement starts at 27 8C. During
of h ¼ 10 cP, even without extra heating of the nozzle plate.
the experiment, the temperature is raised at a rate of
10 8C min1 with a 100 ml min1 dry air gas flow. The
objective of this experiment is to determine two things: the
conditions for the removal of the solvent (blend) and,
secondly, the removal of the capping agent. The TGA-
profile, represented in Fig. 3, shows a distinct mass loss
around 170 8C (blue curve). This can be related to the
removal of the high-boiling solvent, supported by the

Table 1 Sheet resistance of the inkjet-printed silver samples that

are heated up in ambient conditions at a rate of 10 8C min1.
maximum temperature (8C) sheet resistance (mV/sq)

50 1
100 1
150 1
200 1
250 1
300 56
Figure 3 DTA measurement of the JS-B30G silver ink. The blue 350 48
curve represents the mass change, the green one shows the heat 400 40
flow.

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Figure 4 AFM images of inkjet-printed silver nanoparticle inks. The samples are positioned in a box oven under ambient
conditions and are heated up at 10 8C min1. Every sample is taken out at a different temperature ranging from 50 to 400 8C in steps
of 50 8C.

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Phys. Status Solidi A 213, No. 6 (2016)
endothermal signal in the DTA (green curve). Up till about
400 8C, a small decay of mass still occurs due to the removal
of organic compounds in the ink. In literature, it is reported
that pure PVP starts decomposing at 380 8C [26].
In addition, an increase of heat flow can be observed in
the DTA measurements at approximately 400 8C, indicating
that around this temperature the capping agent is decom-
posed oxidatively. No more loss in mass occurs with
further increase of temperature, so one can conclude that
the solvents and the capping agents are removed from the
printed layer. To gain more insight in the influence of
this sintering procedure on the electrical conductivity and
morphological properties, a series of 5 by 5 mm silver
squares is printed on glass slides and heated in a box oven. In
ambient conditions, the samples are heated from room
temperature with a heating rate of 10 8C min1. Every time a
multiple of 50 8C is reached, a sample is taken out of the
oven. All eight samples are subjected to sheet resistance
measurements and AFM (Fig. 4). As shown in Table 1, no
electrical conductivity is obtained until a temperature of
300 8C is reached. The sheet resistance shows a standard
deviation of less than 1%.
This proves that solvent removal by itself is insufficient
to gain electrically conducting layers, since no solvent is
represented at the AFM-picture of the 250 8C sample and no
conductivity can be measured on this sample. Once the
capping agent is removed, sintering occurs causing a
resistivity drop directly below 100 mV/sq. AFM pictures are
taken to get a better understanding why the printed silver
layers start to become electrically conductive only starting
from 300 8C. As can be observed by the first sample
(100 8C), an image with no height contrast is obtained
indicating that the sample’s surface is so smooth that
differences in height cannot be determined via these AFM
measurements.
This illustrates the presence of organic residues on top
of the sample, since the silver nanoparticles cannot be
sintered together yet. When the temperature increases
further (200 8C), the contrast in the AFM images becomes
higher, proving that the solvent layer thickness is
decreasing. At 200 8C, one can start observing nano-
particles. At 250 8C only (capped) silver nanoparticles
remain, which is in accordance with the DTA results. The
size of those particles ranges from 10 to 40 nm, which
matches perfectly with the TEM image in Fig. 2. Since no
electrical conductivity is recorded at this temperature and
the particle sizes are still the same as before the printing, one
may assume that the capping layer is still present at this
temperature. Once the temperature rises above 300 8C,
sintering of the particles can be observed. The higher the
temperature, the larger the grains that are formed. Hence, the
amount of grain boundaries is decreased causing a higher
electrical conductivity.
3.5 Optimisation of the thermal sintering
procedure In conventional inkjet printing, the layers are
not heated gradually, but treated isothermally at a fixed time.
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Hence, silver squares of 10 mm each are printed with a drop
spacing of 10 or 15 mm to find the optimal sintering
temperature and sintering time. Those samples are exposed
to temperatures of 180, 200, 250 and 300 8C during 300 , 600
or 900 . Sheet resistance measurements as well as profilom-
etry are performed on those samples. Samples sintered
below 180 8C and for shorter times than 30 min did not show
any sheet resistance in the range useful for further
applications. For each data point in the figure below several
samples are printed. The sheet resistance of each sample is
measured five times. The standard deviation on every sheet
resistance value is less than 1%.
The results of the sheet resistance measurements are
presented in Fig. 5. The patterns printed with a drop spacing
of 10 mm (solid line) can be observed to have a lower sheet
resistance than the ones with a drop spacing of 15 mm (dash-
dotted line), which is as expected, since the lower the drop
spacing, the higher the amount of silver per unit of area. For
both drop spacings, no significant influence of time on the
sheet resistance is observed in the time interval tested,
except for the ones sintered at 180 8C. Those latter patterns
are both non-conductive after 30 min, but show conductivity
when sintered for 60 min or more. The sintering temperature
appears to have only a slight influence on the sheet
resistance, but once at 250 8C no significant increase in
conductivity seems to be reached anymore.
Another important property of the printed and sintered
layers is the surface morphology. In order to gain more
information about this, profilometry measurements were
performed. No significant trend in the average roughness of
the samples can be observed, but all values can continuously
about 10 nm or less. Further morphological information is
obtained via scanning electron microscopy images (Fig. 6).
Both samples are printed with a drop spacing of 15 mm and
thermally sintered afterwards during 60 min. The top sample
is treated at 200 8C showing smaller features compared to
Figure 5 Sheet resistance of inkjet-printed and thermally sintered
silver squares. Drop spacings of 10 and 15 mm are used. The
temperature varies from 180, 200, 250 to 300 8C. The samples are
exposed to these temperatures during 30, 60 and 90 min.
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Figure 6 Scanning electron microscopy images of silver squares
printed with a drop spacing of 15 mm and thermally sintered during
60 min. Top: sample sintered at 200 8C. Bottom: sample sintered at
300 8C.
the features of the bottom sample treated at 300 8C. Thus, an
increase in sintering temperatures leads to an increase in
agglomeration and void features and to a small decrease in
sheet resistance (Fig. 5).
Figure 7 Bottom emitting light emitting diode stack.
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Figure 8 Left: inkjet-printed silver grids functioning as bottom
electrodes for light emitting diodes. Right: complete and working
light emitting diode with a silver grid instead of an ITO electrode.
3.6 Applications: OLED electrodes The optimisa-
tion of the printing and post-treatment conditions lead to
electrically well-conducting layers with a very low surface
roughness. This creates the possibility to use those inks in
applications, e.g., as OLED contacts. A stack of a bottom
emitting light emitting diode (BEOLED) is represented in
Fig. 7a.
Those devices are typically produced on glass substrates
coated with an indium tin oxide (ITO) layer. Hereupon a
PEDOT:PSS layer and subsequently the active layer (super
yellow) are spin coated. The calcium/aluminium top electrode
is deposited afterwards via physical vapour disposition.
Containing indium, ITO is getting more expensive. Moreover,
it shows a brittle behaviour as well as a high rigidity causing
easy crack formation. Therefore, an alternative can be found in
metal grids [27], such as silver grids. Silver is not transparent,
however, the electrical conductivity is roughly a thousand
times higher than for ITO. The transparency issue can be
solved by patterning the silver in a grid via inkjet printing as
depicted in Fig. 8 (left) and performed elsewhere for organic
photovoltaic devices [28]. Another important factor is the
surface morphology of the grids printed. For instance, the
roughness has to be as small as possible to prevent defects in
the layers that have to deposited on top. Since the average
roughness of the silver layers in less than 10 nm and the
thickness of the subsequent PEDOT:PSS layer is 30 nm, our
silver layers meet the morphological requirements. When
producing OLEDs in the structure represented in Fig. 7b, the
properties of these silver grids are sufficient allowing to
construct a perfectly working OLED, Fig. 8 (right).
4 Conclusions In conclusion, it can be stated that the
ink tested meets the requirements in terms of particle size
and viscosity of the dispersion to be used for inkjet printing.
Furthermore, it is proven via TGA-DTA, AFM and sheet
resistance measurements that the sintering procedure
consists of three important steps. First, the solvents are
evaporated, after which the capping polymer (PVP) starts to
deform once its glass transition temperature is reached.
Sintering of the silver nanoparticles occurs when discarded
from their capping. This results in an electrically conducting
layer with a roughness lower than the particle size of the
capped particles. Because of their high performance, the
inkjet-printed silver layers could be used as an electrode in
an OLED. Further research could be performed on
alternative sintering methods in order to lower the sintering
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Phys. Status Solidi A 213, No. 6 (2016)
temperature and subsequently create the possibility to
deposit and sinter capped nanoparticle inks on heat sensitive
substrates or devices.
Acknowledgements The author would like to thank the
financial contribution from the CORNET project POLEOT (IWT-
TETRA-120629), the SIM Soppomþ program and the support
from BOF (BijzonderOnderzoeksFonds) of Hasselt University.
The author would like to thank Huguette Penxten for performing
the viscosity measurements, Bart Ruttens and Christel Willems for
the support during the SEM measurements and Filip Huybrechts
for the language revision.
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