Flexible and Printed Electronics

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 Flex. Print. Electron. 8 (2023) 025014 https://doi.org/10.1088/2058-8585/acd402

Flexible and Printed Electronics

PAPER

Improved fatigue resistance in transfer-printed flexible circuits

OPEN ACCESS
embedded in polymer substrates with low melting temperatures
RECEIVED
14 February 2023 Thomas Chalklen1, Michael Smith1 and Sohini Kar-Narayan∗
REVISED
Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS, United
26 April 2023
Kingdom
1
ACCEPTED FOR PUBLICATION These authors contributed equally.
10 May 2023 ∗
Author to whom any correspondence should be addressed.
PUBLISHED
30 May 2023 E-mail: sk568@cam.ac.uk

Keywords: aerosol-jet printing, flexible electronics, metallic nanoparticulate ink, fatigue resistance, transfer printing
Original content from
this work may be used
Supplementary material for this article is available online
under the terms of the
Creative Commons
Attribution 4.0 licence.
Any further distribution Abstract
of this work must Flexible electronics are of great interest and importance due to their applications in a range of
maintain attribution to
the author(s) and the title fields, from wearable electronics to solar cells. Whilst resolutions of printed flexible electronics
of the work, journal
citation and DOI. have been improving in recent years, there remain problems with mechanical fatigue and substrate
cost, curtailing the use of such devices and resulting in increased cost and waste products. Here we
present a novel method for improving the fatigue resistance of printed flexible electronics by a
factor of ∼40 by sintering the electronics prior to transferring them into low-cost polymer
substrates, such that they remain embedded. This method is demonstrated using circuits printed
using silver nanoparticulate ink with an aerosol jet printer, and could be applicable to multiple
different metallic inks. At the same time, this method can be used to transfer print circuits into
polymers with low melting temperatures, without the need for otherwise detrimentally high
sintering temperatures required for ink curing.

1. Introduction [11, 17, 18], polymers [19], metallic inks [13, 20–22]
and nanofibers [23]. These materials are usually
Flexible electronics have gained significant interest in deposited upon a flexible, usually polymeric substrate
recent years [1, 2], partly due to the rise in personal and provide low stiffness due to their low thickness,
electronic devices such as folding phones [3], wear- which reduces their second moment of area. This
able electronics and skin inspired electronics [4–6]. flexibility can be improved through geometrical tail-
One of the great advantages of flexible electronics is oring of the electrode structure through the use of
the potential scalability of manufacture. The world is serpentines [13, 24], pre-strained buckling [24–26]
currently facing a global silicon shortage [7], in part and mesh based structures [2, 26].
due to the slow batch processing for silicon electronics A major issue with most such printed electron-
[8, 9]. Owing to their flexible substrates, flexible elec- ics is that they are based on metallic conductive
tronics offer what is called ‘roll-to-roll’ manufacture, inks [27, 28] which require post-deposition sinter-
in a continuous rotating fabrication process [9–12]. ing. Sintering is a relatively high temperature process,
This has significant advantages over batch produc- which is often incompatible with the majority of poly-
tion in terms of cost and scalability, which may help mers due to melting, softening or possible degrada-
to solve significant shortages. However, flexible elec- tion of the polymers at typical sintering temperatures
tronics currently struggle to achieve the resolution (∼200 ◦ C). Attention is turning towards methods
that has been developed in the silicon industry [4, 9]. of preparing low sintering temperature inks to avoid
There is currently significant interest in novel these issues. These methods include the use of solu-
types of flexible and stretchable electronics [2, 4, 13, tion based inks, light based sintering methods and
14] including new materials, such as: paper based forming different complexes of metal nanoparticles
electronics [15, 16], graphene and carbon nanotubes [29, 30]. However, sintering temperatures of 150 ◦ C

© 2023 The Author(s). Published by IOP Publishing Ltd

Flex. Print. Electron. 8 (2023) 025014 T Chalklen et al

are still required even with such techniques. There are but not for connections between different parts of
therefore relatively few polymers suitable as substrates a circuit, although it is feasible that printing meth-
for printed electronics, so commonly polyimide is ods may enable complete circuit production. Another
used due to its thermal stability [6]. However, this approach by Frisbie et al have been based on reduc-
has drawbacks as polyimide is a relatively expensive tion of copper based solutions using printed silver as
polymer (see supplementary table 1) which limits the a catalyst [45–48]. This approach does enable relat-
potential applications of existing flexible electronics ively robust connections to be formed, however it has
due to the prohibitive associated cost of the material. limitations, as photolithographic techniques are used
Furthermore, it is unsuitable for applications requir- to form the initial master pattern for formation of the
ing transparent substrates. A viable method of using substrate, which increases the cost and difficulty of
low cost polymer substrates for flexible electronics the process, as well as introducing a need for align-
would open up novel new applications, such as envir- ment of substrate and print.
onmental sensors including moisture sensors and There remain challenges to be solved in order
even internet-of-things linked sensors [31]. to produce mechanically reliable flexible electron-
Another major difficulty arises from the mech- ics, particularly at a low enough cost for dispos-
anical reliability of the flexible electronics, which able sensors. In this work, by separating the elec-
remains a significant issue for the electronics industry tronics sintering from the substrate, we present a
due to the associated wastage and cost of replacement novel method to embed aerosol-jet printed silver
[32]. Part of the problem is that transferred or prin- based electronics into low-cost polymer substrates.
ted flexible electronic materials remain on the surface The resultant circuits are both flexible and wear resist-
of the substrate, and are therefore more exposed and ant, with fatigue lifetimes more than 40 times longer
susceptible to damage. In addition, bending and flex- than conventionally printed circuits. This method is
ing to relatively small of curvatures is a key feature shown to be compatible with a range of substrates and
of flexible electronics, which exposes the circuitry to able to transfer complex designs into each polymer.
fatigue damage [1, 33–36].
There is therefore a lot of interest in improving
the mechanical behaviour of flexible circuitry [1, 37]. 2. Methods
One method to improve fatigue resistance is to reduce
the thickness of the substrate, as this places the con- Aerosol jet printing (AJP) was used to produce the
ductor closer to the neutral axis, where it experi- transferable circuits in this work with an Optomec
ences lower stresses and is therefore less vulnerable AJ200 aerosol jet printer. Circuitry was printed via a
to fatigue [37, 38]. Another possibility is to embed silver nanoparticle (Ag NP) ink (Prelect TPS 50 G2,
the conductive material inside the substrate, as this Clariant, diluted 1:1 with de-ionised water) as dis-
again moves it closer to the neutral axis, reducing the cussed previously [49]. The Ag NP ink was printed
stress it experiences [4]. This has the added bene- onto an aluminium foil substrate according to designs
fit of reducing the surface exposure of the conductor created in Autocad 2019. Following deposition the ink
to wear and tear. For electronics that are embedded was cured on the aluminium foil by heating to 200 ◦ C
there remain some issues, chiefly that the encapsula- for 2 h. After curing, the foil was wrapped around a
tion process can result in poor contact between the glass slide, with the circuit on the exposed surface as
conducting material and substrate [17]. As a result, shown in figure 1, without the need for post-transfer
effective encapsulation of flexible electronics is gain- high temperature sintering. The glass slide was placed
ing increased attention, primarily due to the envir- onto a custom made stainless steel heating block with
onmental protection it offers [24, 39], but also due an internal k-type thermocouple that is accurate to
to the range of functionalities that are made possible ∼1 ◦ C, alongside a clean glass slide. Pellets of selec-
through the properties of the embedding polymer ted polymers were placed on top of the circuitry and
[40]. the temperature raised to approximately 30 ◦ C above
Some approaches to this have already been tried. the melting point of the polymer, as described in sup-
Several successful attempts have been made to embed plementary table 1. The clean glass slide was posi-
silver nanowires into different substrates via solutions tioned above the polymer melt and was approxim-
of flexible polymers [41–43]. This approach is effect- ately 100 kPa of pressure was applied by hand to cre-
ive due to the high surface area to volume ratio of ate a film of polymer over the printed circuitry. The
the silver nanowires and could be compatible with samples were then removed from the heating block
existing methods of printing for silver nanowires [44]. and allowed to cool, which allows the polymer to
However, there are a couple of drawbacks: firstly, encapsulate the printed circuit. Then the aluminium
the weight loading of both the nanowires and the foil was peeled off the polymer, leaving behind an
solutions are very low (typically less than 1%), res- embedded circuit, as shown in figure 1. Suitable elec-
ulting in low deposition rates and large wastages of trodes may then be attached to the surface using
solvent. Secondly the drop casting and spin coating silver conductive paint to connect to an external
used here are effective for the production of films controller.

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Flex. Print. Electron. 8 (2023) 025014 T Chalklen et al

Figure 1. (a) Schematic of the electrode transfer method. (i) Aerosol jet printing of silver ink onto Al foil. (ii) Arrangement of
materials for electrode transfer. (iii) Melt pressing of polymer. (iv) Removal of glass and Al foil to leave embedded silver electrodes
in polymer. (b) Example of melt transferred silver into polyethylene terephalate showing the University of Cambridge logo. (c)
SEM image of embedded silver lines, consisting of, from left to right: 1, 2, 4, 8, 16 and 32 layers of printed silver. The 32 layer
sample collapsed under the pressure of the gas flow during printing.

Free arc bending tests were carried out as found to increase over multiple cycles (figures 2(d)
described in figure 2(a) and Yi et al [1]. Each bending and (e)).
sample consisted of three separate parallel lines, each Rubbing tests were carried out using a custom
with contact pads to enable four-point resistance linear motor set up. A custom circuit (shown in
measurements. The same design was printed onto figure 3) was printed using the aerosol jet printer onto
Kapton sheet and separately onto aluminium foil. both polyimide sheet (125 µm, Goodfellow) and alu-
The circuit was transferred from the foil into a melt minium foil. The circuit on foil was transferred into
of poly-l-lactic acid (PLA, molecular weight 85000– a melt of polyvinylidene fluoride as described above.
160000, Sigma Aldrich) as shown in figure 1(a). Both The circuit consisted of eight parallel traces, connec-
Kapton circuits and PLA circuits were attached to ted at one end to a common voltage source and to
a linear motor that could oscillate between set dis- separate Arduino input pins at the other. The sample
tances of 42 mm and 28 mm, enabling the circuits was fixed to a glass slide with adhesive and then posi-
to move between flexion and extension as shown in tioned in the linear motor set up. A hardened chrome
figures 2(a) and (b). The flexion induces a peak radius steel ball (5 mm diameter) was positioned above the
of curvature of ∼6 mm, which, according to a beam sample, and repeatedly dragged across the eight prin-
bending analysis using the Euler–Bernoulli equation ted traces at 2 Hz with a normal force of 2 N (assum-
[50], this would suggest a peak strain of ∼1.2% for ing a coefficient of friction, µ of ∼0.2, this corres-
the conventional samples and approximately 0.6% ponds to a frictional force of about 0.4 N). Contact
for the embedded samples. The resistance of each pads either side of the test traces detect each pass
printed line was continuously monitored using a of the ball bearing, allowing a the Arduino to count
four-point measurement (Kiethley sourcemeter). A the number of cycles (as shown in figure 3(a)). After
2% increase in resistance was used as a failure cri- each cycle, the input pins connected to each test trace
terion. This value is sufficiently high so as not to are poled, detecting if the circuit is still intact or if
be affected by system noise, but also not so large the conducting path has been broken. The lifetime of
that tests require an unreasonable time to complete. each printed trace is taken as the number of cycles
A total of 5 samples of each type were tested, each before the open circuit condition is reached. A total
with 3 printed traces, giving 15 measurements for of 4 samples of each type were tested, each with 8
both transferred and conventional methods. This printed traces, giving a total of 32 lifetime measure-
enables a reliable method of measuring the durabil- ments. Scanning electron microscopy images were
ity of the circuit, as the resistance of the circuit was taken using a Hitachi TM3030Plus.

3
Flex. Print. Electron. 8 (2023) 025014 T Chalklen et al

Figure 2. (a) Schematic of mechanical testing of bending test sample during flexion and full extension. (b) A photo of the bending
sample (c) box and whisker plot of the lifetime of bending test samples (defined as the number of cycles to reach 1.02 × R0 ), box
and line represent the 25th percentile, median and 75th percentile, the square represents the mean and the whiskers the upper and
lower bounds. (d) Increase in normalised resistance over repeated bending cycles. (e) Increase in normalised resistance over many
cycles, showing an arbitrarily chosen failure threshold of 1.02 × R0 .

3. Results where it is exposed to smaller strains than on the sur-

face, as is the case in conventional printed electronics.
AJP printed silver ink on aluminium foil was found The effect of the printed trace height (thickness)
to be suitable for transfer, via the method described on effective transfer is shown in figure 1(c). The
in section 2, to a range of polymer substrates, as maximum line thickness successfully transferred was
described in supplementary table 1. The transfer ∼100 µm, as greater thicknesses collapsed under pres-
method presented in this work is therefore compat- sure of the gas flow during printing. However greater
ible with a range of polymers which would not sur- thicknesses may be achievable with a smaller aspect
vive the high temperatures required to sinter the Ag ratios of prints (increased width) or different inks.
NP ink without this method. When transferred into a Supplementary figures 4 and 5 also demonstrate that
polymer, the printed silver is encapsulated, with only the overspray associated with aerosol jet printing is
the bottom surface of the print exposed, as shown also susceptible to transferring into the polymer sub-
in figure 1(b). The encapsulation process largely pro- strate, which may limit the achievable resolution.
tects the printed silver from exposure to wear, as only In order to test the flexibility of the transferred cir-
the surface remains exposed to damage. Furthermore, cuits, free arc bending tests were carried out as shown
the encapsulation of the silver in a thin layer of poly- in figure 2(a). Circuits printed directly onto polyim-
mer may reduce the thickness of a device, and pos- ide and those transferred from aluminium foil into
ition the silver closer to the neutral axis of bending, PLA were compared. The resistance of the printed

4
Flex. Print. Electron. 8 (2023) 025014 T Chalklen et al

lines was measured during oscillation between exten- polymer is sufficiently strong to prevent debonding.
sion and compression as shown in figure 2(d). Bend- The distribution of sample failures for rubbing tests
ing tests were found to increase resistance under conducted on conventionally printed samples and
compression (with the electrodes under strain) and embedded printed samples is shown in supplement-
decrease again during extension, with the electrodes ary figure 3. The embedded samples had ∼40 times
once again relaxed due to the formation of micro- greater mean lifespan than the conventionally prin-
cracks within the printed silver lines (supplement- ted samples (1820 cycles compared to 45). Further-
ary figure 2). Over the course of hundreds to thou- more, both the mean and median of the populations
sands of cycles the resistance increased across the were found to be significantly different at the 1% level
cycle, as shown in figure 2(e). This enables resist- (two sample t test, p = 2.67 × 10−27 , Mood’s median
ance to be used as a measure of the lifetime of the test, p = 5.24 × 10−14 ). For the embedded samples the
samples. The failure point may be defined in mul- silver can still be damaged, yet it is not vulnerable to
tiple different ways [51, 52], however, it is common complete removal (figures 3(d)(iv) and supplement-
for the failure threshold to be defined at some value ary figure 4). From figures 3(d)(iv) and supplement-
of normalised resistance [37, 51–53]. In this work we ary figure 4 it is also possible to observe that in the
have defined the failure threshold to be when the res- embedded sample, wear of the surface leads to redis-
istance of a sample, R, reaches 1.02 times the ini- tribution of silver into the surrounding area.
tial resistance, R0 , thus allowing comparison between In addition, the lifetime of the prints was found
samples with varying values of R0 . This threshold was to increase with increasing layer thickness, as shown
chosen as it represents a reasonable increase in res- in supplementary figure 5. This increase plateaued at
istance that can be achieved within the timeframe greater thicknesses of print, this is likely due to the
of the experiments, and that still differentiates well aspect ratio becoming significant and therefore the
between samples. The distribution of sample failures wear tending to a limiting value. The resistance of
for bending tests conducted on conventionally prin- the printed lines was found to decrease inversely with
ted samples and embedded printed samples is shown the number of print layers (equivalent to area) and
in supplementary figure 1. increase linearly with length according to Pouillet’s
It was found that the embedded silver had ∼50 law [54], as shown in supplementary figure 6.
times the mean lifespan of the conventional prin-
ted silver (5340 cycles compared to 98), as can be 4. Discussion
seen in figure 2(c). The means and medians of
the populations were tested and found to be sig- The applications of the transfer technique presen-
nificantly different at the 1% level (two sample ted above are wide ranging. It is perfectly feasible to
t test, p = 3.57 × 10−13 , Mood’s median test, replace the majority of flexible electronics manufac-
p = 8.39 × 10−7 ). Supplementary figure 2 demon- ture, which are usually based on printing [9], with this
strates the failure mechanism of these samples, with low cost technique, with relatively small changes in
hairline cracks forming perpendicular to the bending manufacturing processes. This would help to prevent
direction. The hairline cracks were the main visible debonding, which remains a major issue for flexible
evidence of fatigue and are likely to be responsible electronics [36], as well as improve the fatigue res-
for the increase in resistance associated with sample istance of manufactured devices, which is currently
failure, although in the embedded samples, failure of lacking. One of the major advantages of the method
the substrate itself is likely to be a contributing factor, presented here is the separation of sintering from the
as in supplementary figure 2(c); this may be due to end substrate. By curing the silver ink on the alu-
the decreased flexibility of the PLA compared to the minium foil prior to transfer, low melting point, low
Kapton sheet. cost polymers, for instance polyethylene, may be used
Following bending tests, rubbing tests were also as the substrate instead of costly high temperature
carried out to examine the wear resistance of the polymers such as polyimide. Furthermore, this will
embedded electrodes in response to surface damage. also reduce the requirement for inks designed for low
These tests were conducted in the manner shown temperature sintering, which are often expensive. As
in figure 3(a), and as described in the methods, a result, this process could also enable a variety of
with a steel ball being used to provide the wear. new devices to be implemented which would not have
The results of the tests are shown in figures 3(c) been possible before due to prohibitive cost [5]. Novel
and (d). In the conventionally printed sample, as sensors may also be designed to utilise the proper-
a result of the printed silver rising above the sur- ties of the given polymer base. For example, a soluble
face of the substrate (figures 3(d)(i)), rubbing even- polymer base may be used to create low cost, flexible
tually causes debonding at the interface between moisture sensors. As the polymer dissolves, the cir-
the silver and substrate, which results in complete cuit will be released and quickly break down, turning
removal of the silver in the vicinity of the con- off the current through the circuit. This could have
tact area (figures 3(d)(ii)). Whereas, in the embed- applications in moisture sensitive areas, such as in
ded sample, the adhesion between the silver and food and chemical storage [31], similar devices could

5
Flex. Print. Electron. 8 (2023) 025014 T Chalklen et al

Figure 3. (a) Schematic of rubbing test, 200 g mass provides a downwards force on a ball bearing which oscillates between two
electrical contacts. Wearing of the printed lines eventually causes an open circuit with no current flowing. (b) Schematic of (left)
conventional printed electronics and (right) embedded electronics, the embedded lines remain closer to the neutral axis during
bending and are less exposed to damage during rubbing. (c) Box and whisker plot of the lifetime of rubbing test samples (cycles
before an open circuit is detected), box and line represent the 25th percentile, median and 75th percentile, the square represents
the mean and the whiskers the upper and lower bounds. (d) SEM images of rubbing test samples. (i) Top down view of
conventionally printed sample before testing and (ii) after failure at ∼80 cycles. (iii) Cross section of transferred embedded
sample before testing and (iv) after failure at ∼3000 cycles.

also be produced with sensitivity to certain solvents, factors governing the success of a given transfer: (i)
or others may utilise UV sensitivity to determine the surface energies of the polymer-silver interface
sunlight exposure. Furthermore, transparent polymer and silver-aluminium interface; (ii) relative thermal
substrates could be used in applications where this expansion coefficients of silver and polymer; (iii) the
may be a requirement. melting point of the polymer; and (iv) the viscosity of
One question that remains, is why the novel trans- the polymer during melting.
fer method presented here is successful with a vari- The relative surface energies of the polymer and
ety of different polymers, but not all. Certain poly- aluminium interfaces are likely to have an effect as
mers are able to encapsulate silver effectively and they will determine the adhesion of the different
de-bond it from the aluminium foil substrate while components. The combination of melting point and
others remain attached. There are several important thermal expansion coefficient is also likely to play a

6
Flex. Print. Electron. 8 (2023) 025014 T Chalklen et al

role, as a greater contraction when cooling from the ORCID iDs

melt will cause residual stresses, which may provide a
stronger frictional force between the silver and poly- Thomas Chalklen  https://orcid.org/0000-0003-
mer. Finally the melt viscosity is also likely to be 2784-9955
important, as this will affect the contact area of the Michael Smith  https://orcid.org/0000-0003-0270-
polymer-silver interface, with a low viscosity melt 9438
forming a greater contact with the surface. Supple- Sohini Kar-Narayan  https://orcid.org/0000-0002-
mentary table 1 shows values for the surface energies, 8151-1616
thermal expansion coefficient and melting point of
various polymers. There appears to be little in the way References
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