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Inkjet Printing of Reactive Silver Ink on Textiles

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DOI: 10.1021/acsami.8b18231

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Inkjet Printing of Reactive Silver Ink on Textiles

Hasan Shahariar,† Inhwan Kim,† Henry Soewardiman,‡ and Jesse S. Jur*,†
†
Fiber and Polymer Science Program and ‡Mechanical and Aerospace Engineering, NC State University, Raleigh, North Carolina
27606, United States
*
S Supporting Information

ABSTRACT: Inkjet printing of functional inks on textiles to

embed passive electronics devices and sensors is a novel
approach in the space of wearable electronic textiles.
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However, achieving functionality such as conductivity by

Downloaded via NORTH CAROLINA STATE UNIV on January 29, 2019 at 17:05:33 (UTC).

inkjet printing on textiles is challenged by the porosity and

surface roughness of textiles. Nanoparticle-based conductive
inks frequently cause blockage/clogging of inkjet printer
nozzles, making it a less than ideal method for applying these
functional materials. It is also very challenging to create a
conformal conductive coating and achieve electrically
conductive percolation with the inkjet printing of metal
nanoparticle inks on rough and porous textile and paper
substrates. Herein, a novel reliable and conformal inkjet
printing process is demonstrated for printing particle-free reactive silver ink on uncoated polyester textile knit, woven, and
nonwoven fabrics. The particle-free functional ink can conformally coat individual fibers to create a conductive network within
the textile structure without changing the feel, texture, durability, and mechanical behavior of the textile. It was found that the
conductivity and the resolution of the inkjet-printed tracks are directly related with the packing and the tightness of fabric
structures and fiber sizes of the fabrics. It is noteworthy that the electrical conductivity of the inkjet-printed conductive coating
on pristine polyethylene terephthalate fibers is improved by an order of magnitude by in situ heat-curing of the textile surface
during printing as the in situ heat-curing process minimizes the wicking of the ink into the textile structures. A minimum sheet
resistance of 0.2 ± 0.025 and 0.9 ± 0.02 Ω/□ on polyester woven and polyester knit fabrics is achieved, respectively. These
findings aim to advance E-textile product design through integration of inkjet printing as a low-cost, scalable, and automated
manufacturing process.
KEYWORDS: E-textiles, inkjet printing, particle-free reactive ink, silver coating, conductive pattern, bending, washability

■ INTRODUCTION
Electronic textiles (E-textiles) have gained great interest in
research, especially for wearable applications.1−5 The adoption
of new materials, machines, and processes that are required for
E-textile manufacturing is challenging the manufacturing
growth of this sector. Of particular concern is the need for a
facile patterning process for developing complex electronic
architectures on textiles. While standard dip-coating processing
of the textile in conductive material solutions can easily
incorporate conductivity in textiles,6,7 it is challenging to create
conductive patterns on textile by this process. Printing
technology is observed as a facile process for physically
integrating heterogenous material on textiles. In particular,
screen-printing has already been adopted to print electronics
on textiles by depositing thick-paste metal inks.8−11 Screen-
printing is widely used for fast prototyping methods to develop
sensors12,13 and other electronics14,15 onto various sub-
strates16,17 but has significant limitations. Screen-printing
requires multiple processing steps, and the viscous pastes
result in a great amount of ink waste and postprocess cleaning
of the screen. The thick pastes used in screen printing also alter
the properties of textile substrates, which change the feel of
textiles. The screen-printed conductive thick paste can easily
crack and lose the functionality by the mechanical deformation
of textiles. Thus, a film lamination or thick surface-smoothing
coating is required to screen-print conductive pastes on
textiles. The use of conductive yarn for making conductive
patterns on textiles also requires multiple expensive processing
steps such as metallization of yarn followed by the mechanical
incorporation (sewing and embroidery) of the conductive
yarns to locally place a functional pattern on textiles. On the
contrary, inkjet printing is a single step automated manufactur-
ing process, which uses much less ink than that of screen-
printing and can deposit a thin layer of conductive or
functional layers on a select pattern region of a surface. Figure
1 shows a comparative analysis of processing steps required in
conductive yarn-based knitting process, embroidery, and
sewing process with the single-step inkjet printing process
for metalizing textile patterns. Inkjet printing processes require
very dilute and low volume functional fluids to continuously jet
Received: October 18, 2018
Accepted: January 15, 2019
Published: January 15, 2019

© XXXX American Chemical Society A DOI: 10.1021/acsami.8b18231

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Figure 1. (a) Different steps for processing existing process of making conductive patterns on fabric using conductive thread/yarn; (b) single-step
process of patterning the conductive structure on textiles by the inkjet printing process.
picoliter-size droplets on the substrates. Primarily, functional
metal nanoparticle inks are used for inkjet printing conductive
patterns on polymeric films and textiles.18,19 Inkjet printing
nanoparticle inks can result in the inkjet printer nozzles to clog,
and thus the inks are limited to sufficiently small particle sizes
in order to flow through the nozzles. Moreover, because of the
high surface roughness and porosity of the textile, a large
number of print passes for high-density metal particles are
needed to create a conductive path20 or, an ink-receptive thick
coating/smoothing layer is required to be deposited on rough
textiles before inkjet printing, thus limiting the soft and pliable
properties of textile materials.21−26 The durability of such
inkjet-printed metal lines on textiles is not well studied and
understood in prior literatures.
Recently, the particle-free reactive metal inks synthesized
using modified Tollen chemistries have shown promising
characteristics, such as achieving high conductivity using low
sintering temperatures (∼100 °C).22,27−29 The conductive
metal exists as a complex ion dissolved in a water-based solvent
system, which only solidifies once heated. Although inkjet
printing of conductive silver nanoparticle ink, reactive ink on
textiles has been reported in the literature,19,25,28 the wetting
mechanism of the diluted ink on the textile fibers, the process
modification of inkjet for porous substrates, and the durability
of the deposited conductive layers have not been well
discussed. The inkjet process was only demonstrated to
deposit functional materials only on the top layer of densely
packed fabric structures, where layers of metal particles added
up on the textile surface to create a conductive network which
might not be durable.18−23,27−29 The modification of inkjet
process was not developed to coat the surface area of
individual fibers in the textile structure. The coating of the
individual fibers around their surfaces in the fabric structure is
required to create conductive percolation in loosely structured
textiles such as knit and to enhance the durability of the
printed layers. Limited research has been performed toward
understanding the process conditions of printing particle-free
inks on textile, particularly toward understanding how to print
on native textiles without any pretreatment coatings to better
facilitate ink reception.
This work utilizes inkjet printing with in situ heat-curing to
deposit reactive silver ink onto various textile substrates
without an interfacial layer. The process was studied by
changing the textile substrate, modifying the number of layers
of reactive ink printed and comparing printing with and
without in situ heating. To print a pattern conformally on
B DOI: 10.1021/acsami.8b18231
Research Article
textile fibers, the ink properties such as viscosity and surface
tension were adjusted with the surface energy of the print
media (textiles) to spread and adhere ink to the surface of the
textile fibers. Additionally, the ink was selected with a sintering
temperature higher than the printer-platen temperature (textile
substrate temperature in in situ heating) during the inkjet
process so that the particle-free reactive ink can adequately wet
the fibers before being solidified. The conductive traces are
analyzed with optical microscopy, scanning electron micros-
copy (SEM) with energy dispersive X-ray spectroscopy (EDS)
mapping, X-ray diffraction (XRD) analysis, and sheet
resistance measurements to determine the conditions neces-
sary to inkjet-print conductive pathways. Furthermore,
validation of the conductive coating applicability to withstand
the common conditions of textile use (mechanical deforma-
tions and washability) is presented.
■
EXPERIMENTAL SECTION
The particle-free conductive ink is a class of commercially available
organometallic reactive compounds which are soluble in an aqueous
vehicle. For example, the ink presented in this work is a silver salt in
an aqueous amine solution. At room temperature, the amine
compound can form a dissolvable complex ion with the silver salt
to form a particle-free solution. The reactive metal inks can then react
to form Ag once heated to a temperature when the silver complex can
be reduced, shown in Scheme 1. The other bicomponents of the
Scheme 1. Formation of Silver from the Organometallic
Amine Compound When Exposed to Heat
reaction are released as volatile gases. The general form of the
reaction is shown in Figure 2a. The chain length of R1 and R2 can be
altered to tune the sintering temperature of the ink. In collaboration
with Liquid X Printed Metal, a silver reactive ink with an optimized
sintering temperature of 140 °C was developed for inkjet printing.30,31
The curing temperature should be such that the ink remains stable at
low temperatures to prevent curing at the capillary inkjet nozzle
during firing droplets. At the same time, the sintering temperature
should not be so high as to degrade or burn the polymer-based textile
fibers. It was found that the ink with 140 °C sintering temperature can
be jetted for a prolonged time without any clogging of the inkjet
nozzle. The physical properties of the ink such as surface tension and
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Figure 2. (a−c) Systematic of process flow for inkjet printing with reactive Ag ink on textile surfaces and (d) XRD characterization of inkjet-printed
conductive ink on polyethylene terephthalate (PET) knit compared with pristine knit samples.
viscosity were adjusted and optimized for stable droplet generation.
The physical properties of the reactive silver ink are listed in Table 1.
Table 1. Characteristics of Reactive Ag Ink Used for Inkjet
Printing
ink characteristics specifications
appearance clear, water-based
viscosity (cP) at 25 °C 11
density (g/mL) 1.1−1.3
surface tension (mN/m) 30−34
diaminopropane; metallic (silver) salt; 10−30%; 10−30%;
diaminoethane 10−30%
To demonstrate the robustness of the particle free-based inkjet
processing on textiles, three very different types of textile materials
and structures were studiedplain-woven fabric made with PET
yarns, single jersey knit fabric made with PET yarns and Evolon
nonwoven fabric made with bicomponent PET and polyamide (PA)
fibers. The surface-free energy of the polyethylene terephthalate and
PA are ∼44 and ∼46 mN/m, respectively,32 which is higher than the
surface tension of the reactive silver ink. This helps the reactive ink to
spread onto the PET and PA fibers. Reactive silver ink was also
observed to not appropriately reduce on cellulose-based substrates
(such as cotton) as the abundant −OH groups trap the silver in its
ionic form to prevent metallization. As a result, the reactive silver ink
results in a nonconductive material that is brown in color on cellulosic
material even with extending heating. The polymer types are confined
to polyester and PA because the reactive silver ink has good adhesion
to the surface and functional group of polyester and PA.
Inkjet Printing Process. The experimental setup for printing is
provided in Figure S1 (Supporting Information). Printing was
performed using a Botfactory Squink thermal drop-on-demand inkjet
printer (90 drops-per-inch), with a printing surface area of 127 mm ×
127 mm and an adjustable Z-direction to accommodate for thick
substrates. The ink cartridge, with 12 nozzles, is made from
polycarbonate and has a foam insert to facilitate the printing of
dilute reactive inks but prevents nanoparticle inks from being printed.
The reactive silver ink was deposited into the cartridge using a syringe
C DOI: 10.1021/acsami.8b18231
Research Article
and needle to penetrate the foam. A syringe filter with the porosity of
0.22 μm was used to filter the ink before using for inkjet printing. The
drop volume of the printer was fixed to 35 pL. A rectangular print
pattern of 40 mm × 4 mm was printed on the fabric substrates. Two
different modes of printing were selectively chosen for the experiment
that allowed for an examination printing with and without in situ
heating of the textile substrate. When printing with in situ heating, the
software allows the plate to be heated to 80 °C, on which the
substrate is placed. The number of layers printed was varied from up
to eight print passes, adjustable via the Bot Factory software. After
printing, the printed traces were heat-cured at 140 °C for 300 s.
Herein, samples in which only the final heat-curing process was
performed are denoted as “ex situ”, whereas samples in which an in
situ heating was performed with the final curing process are denoted
as “in situ”. This curing process was recommended by the ink
manufacturer and was done once all layers were printed onto the
textile substrate.
Characterization. Optical transmission microscopy and 3D laser
scanning confocal microscope (Keyence, model VK-X1000) were
used to observe the ink coverage on the textile substrates. To further
analyze the ink microstructure, ink coverage, and the ink conformity
on fibers, printed samples were characterized by scanning electron
microscopy (SEM) with the EDS mode. The fabric samples were
prepared for the cross-sectional SEM images by dipping them in
liquid nitrogen for 5 min followed by bisecting with a sharp razor
blade. The confirmation of reduced metal silver on the fabric samples
was characterized by XRD. Sheet resistances were calculated by
measuring the resistance of each sample using the two-point probe
method and measuring the length and width of each sample.
The electromechanical performance of the printed conductive line
on the PET knit fabric was tested with Instron, (model 5566)
Mechanical Tester. The durability of the conductive tracks was also
analyzed by multiple cycles of washing and drying, following AATCC
61 for accelerated washing.
■ RESULTS AND DISCUSSION
XRD analysis of the inkjet-printed PET knit sample showed
three distinct diffraction peaks at 38.2° and 44.4° in Figure 2d,
which represent the [111] and [200] Miller indices of cubic
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Figure 3. (a) Measured sheet resistances corresponding to the number of layers of reactive silver particle-free reactive ink printed on various
substrates (knit PET, woven PET, and Evolon) with the comparison of in situ and ex situ heat-curing; (b−d) optical images of printed traces on
knit, Evolon, and woven fabric (face and back side) for in situ and ex situ heat-curing process. The scale bar is equivalent to 2 mm.

Figure 4. Transmission optical microscopy at 10× resolution of in situ heat-cured (a−c) Evolon, PET knit, and woven fabrics; (d−f)
corresponding interface areas between the printed and nonprinted par of fabrics.

face-centered silver. The pristine PET knit fabric in Figure 2d
did not show any characteristic silver peaks. No silver oxide
was observed in the XRD analysis. Figure 3a shows the sheet
resistance of the printed lines on all the selected fabric surfaces
with respect to the number of layers of ink printed for both the
in situ and ex situ curing. For the following discussion, Figure
3b−d provides microscopy analysis of various fabrics as
observed from the upper and bottom surfaces after eight inkjet-
printed passes. A key observation from these images is the
D DOI: 10.1021/acsami.8b18231
penetration depth of the final conductive coating with and
without the in situ heating. It can be confirmed from the
images that the in situ heat-curing process helped minimize the
wicking (in both in-plane and through-plane directions) and
improved the printed resolution. Because of the high porosity
and surface roughness, the knit fabric with only ex situ heating
required a higher number of print passes (6 layers) to achieve
low sheet resistance. Evolon demonstrated a generally similar
trend with respect to performance although the increased
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Figure 5. SEM images (a) native Evolon fabric (b) Evolon fabric with ex situ heat-curing (c) Evolon fabric with in situ heat-curing and (d−f) and
(g−i) are the corresponding SEM images on PET knit and woven fabrics showing the silver-coated areas.
compactness of the fiber structure and finer diameter of the
fibers increased the capillary force to allow the ink to flow both
in the in-plane and through-plane directions. The penetration
of the ink in the Z-direction of the fabric thickness disrupted
the electrical percolation network with the same amount of ink
volume used. In contrast, the samples that underwent the
additional in situ curing process resulted in significantly lower
resistance, presumably due to the in situ annealing evaporating
the water-based solvent before the ink penetrates into the
inner textile structure and localizing a thicker conductive
coating on the near surface fibers. On the contrary, increasing
the temperature of the fabric helps improve the wetting
property of the ink as the surface tension and the viscosity of
the ink decreases with temperature,33 which helps coat the
fiber conformally, decrease the sheet resistance and improve
the durability of the printed patterns. In general, it is observed
that the in situ heat-cured traces on Evolon and knit require
fewer print passes to achieve a sheet resistance two orders of
magnitude lower than samples that were just ex situ heat-
cured. This large discrepancy was not observed in the woven
PET samples as the large fiber diameter and the tight fabric
structure (low porosity) of the structure was able to reduce the
overall ink penetration in the fabric, resulting in an increased
percolation network on the surface of the fabric. Thus, the
woven fabric achieved the lowest sheet resistance of about ∼1
Ω/□ after four print passes for both in situ and ex situ heat-
cured procedures. Still, in situ curing process did show some
reduction of the sheet resistance (0.2 Ω/□).
Figure 4 shows the magnified optical images using a 3D laser
confocal microscope of silver traces produced by inkjet
printing of the particle-free reactive inks. It can be seen that
the knit fabric has the most open structure while the Evolon
nonwoven has a very dense, randomly oriented fabric structure.
The woven fabric has a tighter structure than the knit fabric,
and it is constituted with fibers that have a largest diameter
than that of other substrates. All the fabric samples, Evolon
fabric, PET-knit, and woven fabrics seem to have good
coverage of the ink on the surface as observed in Figure 4d−f.
E DOI: 10.1021/acsami.8b18231
Research Article
The edge pattern of the coating, visible in Figure 4d−f
demonstrates that the ink was coated on the fibers of the fabric
without blocking the open structure of the textile fibers. This is
the unique phenomenon of inkjet printing with the particle-
free reactive ink.
Figure 5 shows the SEM images of the inkjet-printed
substrates. The images also compare the ink coverage on the
fibers for the in situ heat-cured and the ex situ heat-cured
samples with a control native fabric (unprinted area). The
comparatively brighter portion of the fibers is the indication of
the silver conductive ink in the SEM images. Figure 5d−f
shows the SEM images of the ink coverage on the Evolon
substrate. Evolon has a more distributed coverage of the ink on
the fibers than that on the fibers of the knit fabric.
Interestingly, the ink resides on the edges of fibers on Evolon
fabrics, shown in both Figure 5b,c. This migration of ink is
possibly due to the cylindrical shape of the fine fibers.
Additionally, the ink areas on Figure 5c correspond to the in
situ heat-cured printed area on Evolon, which seems denser
and more concentrated than the ex situ heat-cured substrate
shown in Figure 5b.
From Figure 5d−f, we can observe that the silver coverage of
the fibers on knit PET substrates is improved with in situ
curing. Furthermore, Figure 5g−i demonstrates that the silver
coverage on the woven fabric is more uniform than that of knit
and Evolon. Additionally, there is not a noticeable visual
difference of ink coverage between the ex situ and in situ cured
samples on the woven fabric. This explains the result in Figure
3a that the sheet resistance of conductive pattern on woven
fabric is very similar for both ex situ and in situ heat-cured
samples.
Figure 6 provides a pictorial representation of how a droplet
is able to spread on cylindrical fibers with different diameters.
In a short summary, the inkjet drop can spread longer in length
on a fiber when the diameter of the fiber is higher than the
droplet and vice versa, given the surface energy of the fibers is
similar. This phenomenon can be further explained by the
following equation34
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Figure 6. (a) Ink droplet tends to move to the junctions of the fibers
when the drop diameter is larger than the fiber diameter; (b) drop can
spread when the fiber diameter is larger than the diameter of the ink
droplet.
K 2 = (x 2 2 − a 2x12)x 2 2
where x1 and x2 are the diameters of the ink drop and the fiber,
a is a constant related to the surface energy of the fiber, and K
is the capillary length. From eq 1, we can see that whenever x1
(drop diameter) < x2 (fiber diameter), the value of the capillary
length of the fluid is higher for a constant wetting behavior of
the fiber surface. As a demonstration of this phenomenon, Fig-
ure 7 shows the detailed orientation of the silver ink on the
surface of fabric using EDS to show the residing location of
silver. The fiber diameter of Evolon varies from 3 to 7 μm,
which is much smaller than the diameter of the ink droplet (32
μm). As a result, the ink mostly resides at the edges and
junctions between the fibers instead of spreading on the
surface of fibers, as shown in Figure 7a,d. It can be predicted
that the drop impacting on the multiple fibers and their
crossover points experience a capillary force (created by the
capillary spacing between fibers) that draws the ink to the fiber
junctions. It is noted that increasing the surface energy and
decreasing the droplet size would help to conformally coat the
fibers with conductive ink. From Figure 7b,c,e,f, it is observed
that the ink drop tends to spread more when impacting the
knit and woven fabric structure. In this case, the larger
diameter of the fibers (∼20−30 μm) is comparable to the ink
droplet size and helps facilitate the spreading of the drop.
One of the great advantages of the particle-free reactive
silver ink over the particle-based is that the porous, cylindrical-
shaped textile fibers can be conformally coated by the inkjet
process. This process is very similar to a dying process, where
the dyes can be coated just on to the fiber surface and can also
Figure 7. SEM images inkjet-printed (a) Evolon nonwoven and (b) PET knit fabric and (c) PET woven fabric; and (d−f) corresponding EDX
images (pink color represents silver).
Research Article
diffuse to the fiber to some extent. When the droplets of the
inkjet nozzles impinge on the fibers, the adjacent droplets of
the particle-free reactive ink settle down on the fiber surfaces,
spread and wet fiber over time, forming conformal films
around the fiber surfaces. These conformal films of the reactive
ink around the fiber surfaces get sintered to form elemental
silver upon the annealing process. The mechanism of creating
conductive pathways with the reactive ink on textiles is
fundamentally different than that of particle-based ink. Figure
S2 in the Supporting Information shows the difference in the
wetting properties of the particle-based and the particle-free
conductive inks in the inkjet printing process. The particle
colloidal system is very different because the density of the ink
is much higher due to high loading of metal nanoparticles.
Thus, the gravitational force is much higher, and the particles
(1)
start filling up the fiber gaps when the ink is printed on the
textile surface.35
Figure 8a,b provides cross-sectional SEM imaging of the
silver coating on the knit and woven fabric, respectively. Both
Figure 8. SEM cross-section of the conformal coating of the Ag ink
during inkjet printing on (a) the woven PET and (b) knit PET
fabrics.
figures show that the silver is conformally coated around the
fiber surfaces without filling the areas spaced among fibers. The
thickness of Ag after seven print passes ranged from 150 nm to
1 μm, which can be influenced by a number of factors
including interlacing points between fibers, fiber’s waviness,
and the porosity in the textile. Thus, inkjet printing with the
particle-free reactive silver ink retains the feel/hand of pristine
textile fabric.
An electromechanical analysis of printed patterns on the
PET knit fabric was performed to understand the change of
mechanical function of the fabric after printing. In this analysis,
the PET woven fabric and Evolon nonwoven is not stretchable
because of the inherent fabric structure. Therefore, only the
F DOI: 10.1021/acsami.8b18231
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Figure 9. (a) IR images (top) of the inkjet-printed knit textiles under tensile tension while applying a dc voltage (1 V) to generate resistive heating
and their optical microscope images (bottom); (b) corresponding graph showing the decrease of the resistance under strain; (c) tensile properties
of the pristine (bare) and inkjet-printed knit textiles; and (d) change of normalized resistance of the inkjet-printed conductive knit over the bending
cycles.

Figure 10. (a) Accelerated washing procedure following AATCC test method 61 and (b) change of resistance for knit (red) and woven (black)
polyester fabric with different washing cycles.

PET knit fabric was examined. An interconnect pattern of 30
mm × 4 mm was printed with seven repeating print passes on
the PET knit fabric. Figure 9a shows the infrared (IR) images
and the optical images of the printed interconnect while it was
stretched to 180% of the initial length (30 mm) using the
Instron mechanical tester. The printed conductive pattern with
interconnects was connected to a power source to generate
resistive joule heating. Additionally, the real time change of the
resistance was recorded when the conductive pattern was
stretched using the digital multimeter. The experimental setup
image is shown in the Supporting Information at Figure S3. It
is noteworthy that the interconnect kept heating when the
fabric was stretched to 100% of the initial length. This proves
the current is flowing through the path of fabric in the
G DOI: 10.1021/acsami.8b18231
stretched condition. The knit loops of the fabric get closer and
create closer pack of conductive fibers, as shown in the optical
images in Figure 9a. This characteristic of the knit structure
helps to decrease the resistance while the knit fabric is
stretched. Figure 9b shows the change of electrical resistance of
the interconnect printed on a knit fabric with the increase of
the strain rate. Figure 9c compares the load-elongation curve
for the pristine knit fabric with inkjet-printed interconnects on
the same fabric. The data clearly suggest that there is no
significant difference in the mechanical properties of textiles
after the demonstrated inkjet printing process. The result
confirms that inkjet printing of the particle-free reactive ink
does not alter the structural and physical properties of textiles
(see demonstration in the Supporting Information). Figure 9d
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shows the change of normalized resistance over 10 000
bending cycles for the inkjet-printed conductive knit. The
fabric was bent in the course direction along the continuous
knit loops. There is no significant increase or change of the
resistance observed over 10 000 bending cycles, which is
unprecedented for printed conductive textiles. This example
confirms a significant advantage of inkjet printing of the
particle-free reactive ink directly on knit textiles (without any
coating or film lamination) over any other process.
Apart from the features such as conductivity, preserving the
comfort of textiles, the wash durability/fastness of the inkjet-
printed conductive patterns on textile fabric is an unavoidable
requirement for many E-textiles applications, but is still rarely
reported following industry standards. Figure 10 shows the
change of resistance of the printed patterns on knit and woven
fabric after 5, 10, 15, 20, and 25 regular wash cycles, following
AATCC test method 61. The fabric swatch is dipped in a
cylindrical canister where 0.24 g of detergent powder is added
in 150 mL of water. Fifty steel balls are also added in the
canister to intensify mechanical agitation. The canister is then
rotated for 45 min at 49 °C water bath in the washing machine.
After the washing process, the sample is rinsed and dried at 50
°C for 15 min. It needs to be mentioned that one accelerated
wash cycle as defined by the method is equivalent to five
regular wash cycles. The conductive pattern on nonwoven
increased the resistance 50 times after a single wash (2.3 Ω ±
0.2 to >100 Ω). The resistance of the conductive pattern on
the knit fabric increased 2 times after 15 regular washing and
drying cycles. After 20 washes, the resistance increased to >1
kΩ. The conductive pattern on the woven fabric showed the
highest wash durability, showing little change through 15
washing cycles. The conductive woven sample showed a
reasonable amount of change of resistance (∼3.5× increase)
after 25 wash cycles. These wash durability results of the inkjet-
printed conductive patterns on the knit, woven, and Evolon
further confirm that the large diameter and high surface area of
fibers in the woven fabric enhance the adhesion of the
conductive ink and hence improve the wash durability. On the
other hand, the concentrated ink portions on to the fiber
junctions on Evolon are loosely attached to the fibers. Thus, it
can be surmised that the ink particles were washed off during
the first wash cycle. The XRD analysis of the washed knit
sample after 15 cycles of washing (Figure S4) does not show
any characteristic peaks of silver oxides, which proves that the
silver layers on the fabric do not oxide even after washing
cycles. The increase of resistance in the washing process may
happen because of the wearing of the silver layer by the
mechanical agitation during the washing process. It can be
summarized that wash durability of the demonstrated inkjet-
printed textiles largely depends on the physical structures of
the fabric. Selection of a tighter structure (less porous) can
result in reduced sheet resistance and wash durability of the
inkjet-printed pattern of the reactive particle-free silver ink on
textiles.
■ CONCLUSIONS
Inkjet printing of the reactive silver ink on knit, woven, and
nonwoven fabrics is demonstrated without applying any
additional surface coating or any modification. The reactive
silver ink chemistry is compatible on the PET and
bicomponent PA and PET polymeric fibers. The particle-free
reactive ink can uniquely coat the textile fibers all over the
surfaces without altering the inherent properties of textiles.
H DOI: 10.1021/acsami.8b18231
Research Article
The conductivity of the printed traces on the selected fabrics
depends on the tightness of the fabric structures, fiber
diameters, porosity, and surface energy. The addition of an
in situ heat-curing during the printing process was shown to
decrease the sheet resistance by two orders of magnitude for
PET knit and Evolon fabric. For compatible textiles with fiber
sizes smaller than the ink droplet, the ink has the tendency to
reside at the junctions of the fibers rather than spreading
longitudinally along the fiber length. However, the cured ink in
the fiber edges and junctions creates a meshlike network to
create a conductive path. Additionally, the inkjet printing of
the reactive silver ink on knit textiles achieved unprecedented
conductivity, bend durability, and wash durability without
changing the comfort and the pristine mechanical properties of
the fabric. This work aims to serve as a future guide for
understanding conductive inkjet printing on textiles through
the specific interjoined ink to textile properties such as a drop
size of inkjet, surface tension, and drop spacing that can
enhance the electrical and durability performance of the
conductive pattern on textiles.
■
*
ASSOCIATED CONTENT
S Supporting Information
The Supporting Information is available free of charge on the
ACS Publications website at DOI: 10.1021/acsami.8b18231.
Demonstration of the inkjet printing process on textiles,
an image showing different wetting behaviors of the
particle-based and particle-free ink of textile fibers during
the inkjet process, an image showing the experimental
setup to analyze the electromechanical and in situ
thermal properties of the inkjet-printed conductive
interconnect on knit textiles, and the XRD analysis of
inkjet-printed conductive textiles before and after the
washing process (PDF)
Demonstrating the inkjet printing action (AVI)
Experiment to evaluate the adhesion silver ink to the
fabric (AVI)
Measuring the resistance of the printed pattern on PET
Knit fabric and conducting a visual inspection of the
printed sample (AVI)
■ AUTHOR INFORMATION
Corresponding Author
*E-mail: jsjur@ncsu.edu.
ORCID
Hasan Shahariar: 0000-0003-4307-0327
Inhwan Kim: 0000-0002-3794-2777
Jesse S. Jur: 0000-0003-0244-8645
Notes
The authors declare no competing financial interest.
■ ACKNOWLEDGMENTS
This work is supported by the US National Science
Foundation through the Nanosystems Engineering Research
Center for Advanced Self-Powered Systems for Integrated
Sensors and Technologies under Grant EEC 1160483. This
work was performed in part at the Analytical Instrumentation
Facility (AIF) at North Carolina State University, which is
supported by the State of North Carolina and the National
Science Foundation (award number ECCS-1542015). The AIF
is a member of the North Carolina Research Triangle
ACS Appl. Mater. Interfaces XXXX, XXX, XXX−XXX
ACS Applied Materials & Interfaces
Nanotechnology Network (RTNN), a site in the National
Nanotechnology Coordinated Infrastructure (NNCI).
■
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