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 Page 1 of 7 Journal of Materials Chemistry C
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DOI: 10.1039/C5TC03679H

A facile way of fabricating flexible and conductive cotton fabric

Sicong Liu, Mingjun Hu, Jun Yang*
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Journal of Materials Chemistry C Accepted Manuscript

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DOI: 10.1039/b000000x [DO NOT ALTER/DELETE THIS TEXT]

Abstract:
There is an increasing interest in the area of conductive textiles, also called e-textile, in both the scientific and industrial field.
Herein, we have successfully prepared a conductive textile via electroless deposition onto cotton textiles by using a three-step
treatment process. The cotton textiles are first dipped in P4VP-SU8 solution to form a uniform layer for the subsequent
absorption of silver ions. Then, the cotton textiles are immersed in silver nitrate solution in preparation for the next step
electroless deposition. Parameters like P4VP concentration and ELD conditions are studied to optimize the whole process.
Compared to other methods, the whole fabrication process is efficient, facile and time-saving. The as-made cotton fabric sample
showed sheet resistance as low as 0.05 Ωsq-1 , which proves this method is a promising candidate for applications in the
fabrication of functional textile-based wearable devices.

Introduction
Wearable and flexible electronics have received significant
attention and can be applied into many fields, such as displays,
solar cells, sensors, energy devices and health-monitoring devices
while maintaining functionality when subject to large stress and
deformation. 1 - 6 Traditional electronic fabrication is largely
dependent on photolithography, a time-consuming and complicated
process that involves large volumes of poisonous waste and
expensive facilities. 7 The new era of electronics is no longer
restricted by rigid board circuits, so textile-based wearable
electronic systems8 hold great promise.
Electronic textiles (e-textiles) have been considered as important
applications in future wearable electronics and smart clothing,
which can combine the functionality of smart electronic devices
9
with the comfort and flexibility of stylish clothing. E-textiles not
only provide wearing comfort, but also can function as pressure
10 11
sensors, electrocardiogram (ECG), electromyography
(EMG), and electroencephalography (EEG) 13 sensors, RFID
12
14 15
tags, supercapacitors etc.
Generally, e-textiles can be readily made by knitting, weaving,
16 17
embroidering, coating/laminating, printing, dip coating, and
18
atomic layer deposition. Commercial conductive threads are
exploited in embroidering, sewing and weaving. Though the
conductivity of traditional conductive threads is pretty good, the
cost and weight is relatively high, and mechanical flexibility is
sacrificed as well. Expensive facilities have to be utilized for
atomic layer deposition, adding to the cost and inconvenience. Dip
coating methods to achieve conductive threads have been proposed
19 20
such as conductive polymers, carbon nanotubes,3 graphene,
21
and metallic nanowires. Dip-coating is quite facile and
convenient, but physical absorption is not as stable as chemical
absorption. What’s more, dip-coating is not suitable for creating
patterns, which limits the utilization.
Other than these techniques, electroless deposition (ELD) is
especially attractive because it does not require expensive
fabrication facilities and can be implemented under ambient
Department of Mechanical and Materials Engineering,
Western University, London, Ontario, N6A 5B9, Canada.
*E-mail: jyang@eng.uwo.ca*
conditions on a large industrial scale.22-25 ELD is an auto-catalytic
technique used to deposit various kinds of metals (copper, nickel,
etc.) on different substrates such as plastic, paper, metal oxide, and
26 28
even yarn. - Zheng’s group have demonstrated the electroless
deposition of copper and nickel onto various textile surfaces to
fabricate electrically conductive textiles in a way that has been
29 33
modified with a thin layer of polyelectrolyte brushes. - However,
their method needs silanization first and then ATRP polymerization,
thereby involving many organic chemicals, harsh experimental
condition and is time-consuming, limiting their applications. We
have developed a more facile and time-saving way to deposit
copper on cotton textiles using an electroless deposition (ELD)
process. Cotton fabric is chosen as the fabric substrate because it is
a more commonly-used textile materials.
In this proposed fabrication method, poly(4-vinyl pyridine)
(P4VP) is first attached to the target textile by dip coating, and
subsequently bonds with silver ions. P4VP is a very attractive
polymer for immobilization of nanoparticles because of the strong
affinity of pyridyl groups to metals and its ability to undergo
34
hydrogen bonding with polar species. Cross-linked SU-8 is well
known for its good physical and chemical properties. 35 It can
work as a cross-linking agent for P4VP and cotton fabric. When
P4VP is mixed with SU-8, pyridine rings of P4VP can start the
process of the polymerization of epoxy groups of SU-8 and thus the
semi-interpenetrating polymer networks between crosslinked epoxy
36 37
and P4VP can form. , The epoxy groups of SU-8 can also
react with hydroxyls groups in cotton, leading to the formation of
38
ether groups. Silver ions absorbed by P4VP have been
demonstrated to be an effective seeding and adhesion layer39 for
subsequent ELD of copper to yield conductive textiles in which the
metal-deposited textiles show excellent mechanical and electrical
properties. Importantly, the whole process is carried out in air and
aqueous environments, which are more compatible with typical
40
roll-to-roll fabrication processes in the textile industry. What’s
more, different kinds of patterns can be directly printed onto the
textiles by techniques such as inkjet printing, and so it meets
different requirements.
 Journal of Materials Chemistry C
Experimental:
Materials:
Poly(4-vinylpyridine)(P4VP, Mw ~60,000), silver
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nitrate(AgNO3,99%,) potassium sodium tartrate tetrahydrate
(C4H4KNaO6•4H2O, 99%), ethylenediaminetetraacetic acid
disodium(C10H14N2O8Na2•2H2O,98%) copper(II) sulfate
pentahydrate (CuSO4•5H2O, 98%), formaldehyde solution (HCHO,
36.5–38% in H2O), 2,2-Dipyridyl(98%) are from
SIGMA-ALDRICH, 1,4-dioxane(CH2CH2OCH2CH2O) and sodium
hydroxide (NaOH, 97%,) both from CALEDON, SU-8(Kayaku
Micro Chem). Liquid Tin is from MG Chemicals. All chemicals are
used without further purification. The cotton fabrics are from a 100%
cotton T-shirt (All-Journey Gear Co. Ltd) bought in Sears without
any pretreatment.
2.2 Surface treatment
The ratio of P4VP and SU-8 is 10:1. 1g P4VP was first dissolved in
25 ml 2-propanol and 250 µL 40% SU-8 was dissolved in 25 ml
dioxane, followed by mixing the two solution together for 3
minutes using a VWR mixer until a clear solution was obtained.
The cotton fabric sample was dipped in the mixture solution for 3
minutes, dried in air, and then was heated in the oven for 15
minutes at 120 °C for cross-linking.
2.3 ELD process
The P4VP-SU8 coated cotton fabric sample was immersed into 2
g/L silver nitrate solution. The sample was rinsed by distilled water
to remove the redundant silver ions after being taken out of the
solution. Electroless deposition was performed in each cotton
fabric sample for 30, 60, 90,120, and 150 min, respectively, in a
solution bath containing a mixture of freshly prepared solution A
and B. Solution A consisted of 28 g /L CuSO4•5H2O, 26 g /L
Fig. 1 gives a systematic illustration of the procedures of fabricating copper-coated cotton fabric. Step 1: pristine cotton fabric and P4VP are connected by
polymeric graft chains containing epoxy groups. Step 2: Silver ions are attached to P4VP because of the affinity of pyridyl groups. Step 3: copper is deposited
onto cotton fabric .
Page 2 of 7
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DOI: 10.1039/C5TC03679H
NaOH, 32 g/ L KNaC4H4O6•4H2O, 40g/L EDTA•2Na, 40mg/L 2,
2-Dipyridyl, and 20mg/L K4Fe(CN)6. Solution B was 52 mLL-1
HCHO in distilled water.
2.4 Characterization
A Hitachi S-4500 field emission scanning electron microscope
Journal of Materials Chemistry C Accepted Manuscript
(SEM) and a Tabletop Microscope TM3030plus were also used to
observe the surface morphologies of the textiles. Fourier transform
infrared spectra (FTIR) were recordedusing FT-IR NICOLET 6700
(Thermo Scientific Co.). The XPS spectra were collected using a
Kratos AXIS Ultra XPS from an area approximately 700*300
microns in size, using a monochromatised AlKα X-ray beam.
Contact angle was measured by Ramé-Hart Model 100 Contact
Angle Goniometer with micro-syringe attachment (manual system).
A four-probe method using an M2750 Keithley Multimeter was
carried out to measure the sheet resistance
Result and discussion:
To initiate the copper reduction, palladium or silver ions are needed
to serve as the catalyst. Instead of using an expensive PdCl2
41
activator, we chose a cheaper AgNO3 activator without affecting
the properties of the Cu-coating. To immobilize silver ions, surface
modification with a functional group is required to provide
attractive interaction to ions or nanoparticles. P4VP has been
proved to be an excellent surface modifier for immobilization due
42
to the strong affinity of pyridyl groups. The network structured
SU-8 is a good cross-linking agent for P4VP and cotton fabric,
making P4VP coating more uniform on cotton fabric. The silver
ions are first reduced by HCHO, then Ag0 acts as a catalyst for the
subsequent Cu deposition in the electroless coating bath,
stimulating copper to act as a self-catalyst in the subsequent
reaction.37
 Page 3 of 7 Journal of Materials Chemistry C
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DOI: 10.1039/C5TC03679H

cotton O 1s
P4VP/SU8 cotton P4VP/SU8 cottom
a P4VP/SU8 cotton after heating b prinstin cotton
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C 1s

Intensity(a.u.)

Journal of Materials Chemistry C Accepted Manuscript

Transmittance
N 1s

500 1000 1500 2000 0 200 400 600 800 1000 1200

Wavenumber (cm )
-1 Binding Energy(eV)

Fig.2 (a) FTIR spectra of pristine cotton, P4VP/SU8 coated cotton, heated P4VP/SU8 coated cotton (b) XPS spectra of P4VP/SU8 coated cotton

Fourier transform infrared spectroscopy (FT-IR) was conducted to
confirm the coating of P4VP and SU8 (Fig. 2a). In both P4VP/SU8
coated cloth and heat treated P4VP/SU8 coated cloth, the intensity
of strong peaks at 1590 cm-1, which are attributed to stretching
vibrations of pyridine peaks, changed after heating.37 It was
possibly because of ring-opening reaction of epoxy groups of SU8
and the reaction between P4VP and SU8.
X-ray photoelectron spectroscopy (XPS) was also conducted to
analyze the surface chemical composition of the pristine cotton and
P4VP/SU-8 coated cotton. Figure 2b and Table S1 shows that the
carbon content in the sample increased, while the oxygen content
decreased after the coating process, during the course of surface
treatment. What’s more, the presence of nitrogen was detected after
surface treatment, confirming the successful absorption of P4VP.
By comparing the C1s spectra of the cotton fabric obtained before
and after surface treatment, the intensity of the C-H/C-C peak was
found to increase after surface treatment, while the intensities of
the O-C-O and C-O peaks are attenuated (see Fig.S3), because the
CH2 and cyclopyridyl contents are increased with the P4VP and
SU8 coating.
A control experiment was conducted to verify the necessity of
surface treatment. One cotton fabric sample was directly immersed
into silver nitrate solution without surface treatment, while the
other was given the treatment. Both samples were then placed in
the copper plating bath for electroless deposition. From the result,
in Fig. S4, it can be obviously seen that the left sample (without
P4VP/SU8 coating) was almost black while the right one (with
P4VP/SU8 coating) had a bright red colour. The colour difference
can be attributed to the extent of silver ions absorption. Silver ions
were physically absorbed by the sample with no coating, while
silver ions were immobilized by the pyridyl groups in the coated
sample. Physical absorption tends to absorb more silver ions than
chemical absorption because of limited pyridyl groups. During the
thus affecting copper plating. The conductivity of cotton fabric
samples in 2 %, 3% and 4% concentration were close. However,
from outward appearances, the copper was distributed uniformly on
the 2% sample and there were some copper clusters formed on the
3% and 4% surface. The higher the P4VP concentration is, the
greater the viscosity of the solution is, and the poorer the fluidity is.
The poor fluidity of P4VP solution may result in the nonuniform
coating on the cotton fabric surface. The formation of copper
clusters may be due to the fact that the catalytic speed is higher in
the place with more P4VP molecules loaded. Conclusively, we
adopted the 2% concentration as the optimal choice.
Although the surface morphologies of P4VP-SU8 coated cotton
and untreated cotton look quite similar, water contact angle
measurement shows their gigantic difference in surface wettability.
Cotton is a hydrophilic natural polymeric material. When a droplet
of water was dropped on the surface, it quickly soaked into the
fabric and disappeared. After the P4VP-SU8 coating, the cotton
fabric surface became quite hydrophobic because P4VP is water
insoluble and SU-8 is hydrophobic. The water contact angle was
110.5°(Fig. 4B). After the ELD process, the surface of the cotton
fabric sample was covered with a layer of uniformly distributed and
densely packed copper particles(Fig.4C’), which was further
proved by energy-dispersive X-ray spectroscopy (EDS) (see Fig.
S2). The EDS analysis also showed that 80% was copper, which
showed that the copper film formed during the ELD process
surrounded every fiber uniformly. After copper deposition, the
surface became hydrophobic again and the contact angle was
95.8°(Fig. 4C).
0.10
sheet resistance
0.09
Ω sq-1)

0.08
ELD process, the excessive silver ions absorbed by the sample with
Sheet Resistance(Ω

0.07
no coating were easily reduced to silver, but they tend to diffuse
into the solution and hardly play as a stable catalytic center for 0.06
immobilization of subsequent fresh copper atoms. The inconsistent 0.05
layer of nano-sized silver particles resulted in the poor conductivity
0.04
of the sample without coating.
To find the best P4VP concentration, four solutions with 0.03
different P4VP concentration ranging from 1% to 4% were 0.02
prepared. The ELD time was set to 90 minutes. The sheet 1 2 3 4
resistance was measured, as shown in Fig. 3. The conductivity of Concentration(g/L)
the cotton fabric sample in the 1% concentration was poor
compared to the other samples. This was because less P4VP means Fig.3 Sheet resistance of copper cotton at different P4VP concentration.
fewer amino groups, where fewer Ag+ moieties were immobilized,
 Journal of Materials Chemistry C Page 4 of 7
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Journal of Materials Chemistry C Accepted Manuscript

Fig.4 SEM images of (A,A’) pristine cotton fabric; (B,B’) P4VP/SU8 coated cotton fabric;(C,C’) copper cotton fabric

0.4
0.14 a weight
b
Electrical Resistance
Sheet Resistance(Ωsq-1)

0.12
0.3

0.10
Weight (g)

0.08
0.2

0.06

0.04 0.1

0.02

0.00 0.0
0 30 60 90 120 150 180 0 30 60 90 120 150 180
Time (Min) Time(Minutes)
2.0

1.9 R/R0 0.90 R/R0

d
1.8
0.85
1.7

1.6 0.80
1.5
R/R0

0.75
R/R0

1.4

1.3 0.70
1.2
0.65
1.1

1.0 0.60

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 0 5 10 15 20 25 30
Stored Time(Days) Bending Radius (mm)

Fig.5 a. Weight gain after ELD at different ELD plating time; b. Sheet resistance of copper cotton at different ELD plating time; c. Resistance aging test of the
copper cotton sample; d. Resistance change test of the copper cotton sample at different bending radius

When we pulled a single yarn from the cotton fabric sample, it from the cotton fabric sample has a much higher resistance. We
can be seen that some parts of the yarn were not fully covered also studied the silver ions distribution at the intersection of
with copper (Fig.S3). It is proposed that the up-and-down cotton fabric sample before ELD process. From the EDS
intercrossed structure of the warp and weft yarns and the analysis result, it can be seen that there are little silver ions
twisting of cotton fibers prohibit the exposure to P4VP. found. The silver ions mainly exist on the surface of cotton
Surfaces exposed to P4VP/SU8 solution are merely allowed the fabric (Table S2). From this, it can be inferred that the
crosslinking reaction, so as the subsequent occurrence of ELD conductivity of the copper-coated fabric mainly relies on the
of copper metal particles.31 As a result, a single yarn pulled closely packed woven structure that makes copper metal
 Page 5 of 7 Journal of Materials Chemistry C
particles tight together closely. As long as the woven structure
is compact, the conductivity of cotton fabric won’t be much
affected.
The weight gained during the ELD process should have been
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proportional to ELD time. It was observed that the weight
increased as a linear function of ELD time (Fig. 5a). The weight
reached 106% of its original weight after 150 min. The sheet
resistance of the copper cotton sample was also studied using a
four-probe measurement, which is a measure of resistance of
thin films. Sheet resistance is a strong function of thickness. To
reduce error, we measured several points on the both sides of
the copper cotton sample and calculated the average as the final
result. We demonstrated the effect of time on sheet resistance
when ELD plating time varied from 30 min, 60 min, 90 min,
120 min and 150 min. The average sheet resistance of the
sample was plotted against ELD plating time, as shown in Fig.
5b. The pristine cotton sample and P4VP-SU8 coated sample
were electrically insulated. After 30 minutes of ELD, the
sample became electrically conductive, but its resistance was as
high as 0.25 Ωsq-1. Most of the surface appearance of the
sample still remained black, which can be explained by the
color of silver particles. The silver particles did not catalyze the
reduction of copper ions fully enough and were still absorbed on
the surface. After 60 minutes, it could be seen that the black
areas decreased dramatically and the sheet resistance decreased
a lot to 0.15Ωsq-1 . When the ELD time was extended to 90
minutes, black areas almost diminished and the color of the
copper cotton sample turned a red copper color. The sheet
resistance decreased to 0.05Ωsq-1 . When the ELD time was
extended to 120 minutes, the sheet resistance decreased to
0.04Ωsq -1 and remained almost the same even for the deposition
longer than 120 minutes, which was consistent with the weight
gain. Considering all factors including efficiency and
conductivity, 90~120 minutes of the ELD is an appropriate time
for copper deposition.
The conductivity change of the copper cotton sample under
aging was evaluated and the sheet resistance of copper cotton (2%
P4VP and 90 min ELD) was recorded when it was stored in air for
a certain amount of time. It was discovered that the sheet resistance
increased by 158% after one day and then remained almost
unchanged for the rest of the next two week proving the long-term
stability, as shown in Fig. 5c. According to the previous study, the
increase in resistance was due to the partial oxidation of Cu into
Cu2O.40 To increase the stability, a layer of air-stable metals, such
as tin, can be capped on top of copper. Liquid Tin is a clear
immersion tin designed and formulated to coat a copper substrate
with a dense tin deposit. The tin deposit owes its outstanding
corrosion protection to its dense coating. After ELD process, the
fabric sample was dipped into the liquid tin solution for one hour,
and a layer of tin was formed because of replacement reaction (Fig.
S5). The sheet resistance of the as-made Sn-Cu cotton fabric was,
however, a little bit lower than the Cu cotton.
The bending test was also conducted to observe the resistance
change. The relationship between the electrical resistance and
different radii of curvature was investigated (Fig. 5d). The
electrical resistance decreased as the bending radius decreased,
which was the same as what Zheng’s group found.40 They pointed
out that when the copper cotton sample is bent to a small radius, the
sample is subject to higher tensile strain, enabling the cotton fibers
and yarns to be stretched to form a more compact contact between
each other, decreasing the contact resistance.
Apart from efficiency and convenience, another great advantage
of this method is that it can print different kinds of functional
View Article Online
DOI: 10.1039/C5TC03679H
patterns on cotton textiles using a normal home use printer. The
inkjet printing method provides benefits like speed, flexibility,
non-contact and creativity. Basically, just a print head and ink are
needed to print whatever you want, like antennas, circuits and other
patterns. Instead of the whole cotton cloth being immersed in silver
Journal of Materials Chemistry C Accepted Manuscript
nitrate solution, patterns can be directly printed using a printer with
silver ink inside after surface treatment. The silver ink used here
was composed of silver nitrate, distilled water and glycerol. First of
all, the cotton cloth was pretreated with P4VP/SU8; Secondly, the
cotton cloth was attached onto a paper for printing silver ink;
Finally, ELD was performed on the cloth for deposition of copper.
As Fig.6a shows, Western University’s logo was printed on a piece
of cotton cloth. For the industrial manufacturing, this method can
also be applied in screen printing on a large scale.
In conclusion, we have proposed a very facile way to prepare
conductive textiles by electroless deposition. This method has
several features that are superior to other methods. Firstly, few
chemicals are used in this method compared to other
methods,43which require lots of organic chemicals, meeting the
demand of green chemistry. Secondly, the whole process can be
completed within 3 hours, which is really time-saving and efficient.
Thirdly, the use of P4VP greatly enhances the absorption of silver
ions onto cotton textiles, facilitating the subsequent ELD process,
and making the sheet resistance as low as 0.05 Ωsq-1. Fourthly,
fabrication of copper-based electronics is achievable on cotton
textile via inkjet printing. Fifthly, the whole fabrication procedures
can be carried out under ambient conditions and is fully compatible
with roll-to-roll processes in the textile industry. Considering the
above advantages, we believe that conductive textiles fabricated by
this method hold remarkable potential and promise towards
production in smart textiles in the future.
A
Fig. 6 a. Western University’s logo printed on cotton fabric; b Passing
current through as-made copper cotton fabric sample to power an LED.
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DOI: 10.1039/C5TC03679H
Published on 12 January 2016. Downloaded by Middle East Technical University (Orta Dogu Teknik U) on 16/01/2016 05:05:50.

Journal of Materials Chemistry C Accepted Manuscript

A facile way of fabricating a highly condutive textile via electroless deposition by just
three steps