Journal of Food Engineering 168 (2016) 79–83

Contents lists available at ScienceDirect

Journal of Food Engineering

journal homepage: www.elsevier.com/locate/jfoodeng

A new type of TTI based on an electrochemical pseudo transistor

Xianglong Wan a,⇑, Meinhard Knoll b
a
Institute of Materials Science and Engineering, Anhui University of Science and Technology, 232001 Huainan, PR China
b
Institut für PhysikalischeChemie, Universität Münster, 48149 Münster, Germany

a r t i c l e i n f o a b s t r a c t

Article history: Conventional time–temperature indicators (TTIs) are usually based on various processes, such as the
Received 18 January 2015 diffusion of colorful solution, color-changing polymerization, enzymatic reactions, and photochromic
Received in revised form 11 June 2015 reactions. In this study, a new type of device based on an electrochemical pseudo-transistor in
Accepted 22 July 2015
structured conductive polymers is presented as a TTI with the activation energy closed to results
Available online 23 July 2015
in other studies and products in market. This TTI provides basic functions, such as clock, tempera-
ture sensor, and electrical switch. Furthermore, this pseudo-transistor-TTI is combined with radio
Keywords:
frequency identification (RFID) technique for the first time. A TTI–RFID label can offer double
Conductive polymer
Electrochemical pseudo-transistor
protection for perishable food by using TTI and RFID readers. This label not only demonstrates that
Activation energy structured conductive polymers can be used as a powerful TTI with an electrical switch but also
Electrical switch supplies a new alternative strategy to combine TTI with an RFID tag to supervise and trace the
TTI–RFID system safety of perishable food.
Ó 2015 Elsevier Ltd. All rights reserved.

1. Introduction
Some perishable products are important to people’s health and
thus should be stored in a chill supply chain (Halm et al., 2010; Lu
et al., 2013). Exposure to high temperature shortens the shelf life,
which is normally marked on the package, of the product. It is dif-
ficult to estimate that the products are still in their shelf life after
exposure to high temperature. Misusing such products may lead to
serious consequences (Techathawat et al., 2007). Time–tempera-
ture indicators (TTIs), which are commonly used on perishable
food to indicate exposure to excessive temperature and time,
operate through different mechanisms to display a best-before
date label. A photochromic reaction (Kreyenschmidt et al., 2010;
Nga et al., 2011), an enzyme (Kim et al., 2012a; Tsoka et al.,
1998; VanLoey et al., 1997) with a reaction or pH indicator (Kim
et al., 2012b; Vaikousi et al., 2009), and nanotechnology
(Zhang et al., 2013) were applied in different TTIs for chilled food
(Kim et al., 2012c; Lee and Shin, 2012; Lu et al., 2013; Simpson
et al., 2012). Most of these TTIs can integrate cumulative time
and temperature history by changing color. Radio frequency
identification (RFID) can be used to store information of food
(Jones et al., 2005; Regattieri et al., 2007), blood products
(Hohberger et al., 2012), or vaccines (Longe et al., 2012) and has
⇑ Corresponding author.
E-mail address: xlwan@ipe.ac.cn (X. Wan).
been used to trace products. Combining TTI with an RFID tag can
be the best choice for products in the chill chain. However, few
TTIs can be integrated with the RFID tag because of the absence
of electrical conduction.
In our earlier works, we have reported that conductive polymer
can be structured as an electrochemical pseudo transistor and used
as an electrical switch (Wan, 2011) in a sandwich structure. The
conductive polymer (activation layer) in the sandwich structure
can be connected directly with an RFID tag. The structure of the
pseudo-transistor is shown in Fig. 1(a). Fig. 1(b) depicts a
pseudo-transistor based on conductive films combined with an
RFID tag.
Polyaniline can exhibit different colors and different conduc-
tance at different states doped by an acid or a base aqueous solu-
tion (Chen and Hwang, 1995; Haba et al., 1999). The aqueous
solution migrates in the blend film with a sharp front (Cohen
and White, 1989; Durning et al., 1995; Nealey et al., 1995) and acti-
vates with the activation layer with a sharp color-changing front.
The color-changing front in polymers is based on chemical doping
(Hermes and Knoll, 2009; Wan and Knoll, 2014) and electrochem-
ical doping (Knoll, 2008; Tehrani et al., 2010). In this study, the
temperature dependency in pseudo-transistor with structured
conductive polymer films and its potential application in a
TTI–RFID device are investigated. The system based on the
electrochemical pseudo-transistor can offer double protection for
perishable products by using TTI and RFID reader.

http://dx.doi.org/10.1016/j.jfoodeng.2015.07.030
0260-8774/Ó 2015 Elsevier Ltd. All rights reserved.
80 X. Wan, M. Knoll / Journal of Food Engineering 168 (2016) 79–83
Fig. 1. Pseudo-transistor based on structured polymer films. (a) Structure of the pseudo-transistor. (b) Transistor system combines with an RFID tag.
2. Material and methods
2.1. Preparation of TTI based on an electrochemical pseudo transistor
This TTI consists of a substrate (polyethylene terephthalate), a
migration layer (hydrophilic polymer), an activation layer (conduc-
tive polymer), two silver contacts on the activation layer, and an
encapsulation (GBCÒ document pouch or clear coating). The activa-
tion layer is prepared from a polyaniline (Panipol Oy, Finland) solu-
tion on the substrate by using a Mayer bar. The migration layer is
coated on the activation layer with a polymer solution blended
with polyvinyl alcohol (PVA, 72,000 g/mol, Carl Roth GmbH + Co.,
Germany) solution (10%, w/w) and 2-hydroxyethyl cellulose
(HEC, 90,000 g/mol, Sigma–Aldrich Corporation, USA) solution
(10%, w/w). The weight ratio of PVA to HEC is 7:3. The thicknesses
of the conductive film and migration film are determined by the
size of the Mayer bar and the solid contents of the solution. In this
study, the dry thicknesses of the conductive film and migration
film are 1.0 and 8.5 lm, respectively. The different layers in this
structure are coated layer by layer and sealed in a pouch. The con-
figuration of the pseudo-transistor with a doping front is shown in
Fig. 1(a).
2.2. Activation and measurements
TTIs can be activated in a NaOH aqueous solution (0.5 M) that
can be sealed in porous materials covered by a thermal sensitive
film. When the temperature reaches a critical value, TTI will be
activated. The color-changing fronts of this chemical doping migra-
tion in this device can be observed by the naked eyes. The migra-
tion lengths are recorded by a camera in a thermostatic cabinet
(AQUALYTIC ET 618-4) at different times and their standard devi-
ations are calculated in four samples. The migration velocities
can be shown as differential migration lengths versus differential
times.
The different tests are simulated in this thermostatic cabinet at
ranged temperature from 0 °C to 40 °C, the accuracy of tempera-
ture is about ±0.5 °C. The activation energy of TTI is calculated by
Arrhenius equation at different temperatures. The performance of
TTI at different temperatures is shown by four samples in the dif-
ferent thermostatic cabinets with appointed temperatures. The
resistance of TTI is measured and recorded by a table multimeter
(UT804, Process Control Equipment, Inc., USA) with a two-probe
method during the experiments. Two probes are connected with
the source and drain in TTI which are fabricated by a silver paste
(Art-Nr. 530042 from Ferro GmbH) during the measurement. And
an RFID tag circle is connected with the TTI (Fig. 1(b)). The changes
of migration length and the corresponding resistance are normal-
ized to the maximum changes. The normalization of migration
lengths and resistances can be compared versus time at room tem-
perature before the label is switched off.
When the TTI–RFID device is in the effective area, it can be read
by an RFID reader. A 13.56 MHz RFID tag with a chip is read by the
RFID reader (USB, ISO15693) to check information regarding the
products. When the device cannot be read, the circle of RFID must
be switched off. It should also be found that the channel is all in
blue by visual inspection at the same time. TTI–RFID device with
13.3 mm activation layer in the channel is checked with changing
temperatures at 5 °C, 10 °C and 23 °C every 25 h. The DC resistance
of the device and migration fronts are recorded until the switch is
turned off. The TTI–RFID device is detected by the RFID reader at
first and after switched off.
3. Results and discussion
3.1. Time dependency in TTI
Fig. 1(a) shows that TTI is structured with a conductive poly-
mer. The conductivity of the activation layer will be determined
by the chemical doping front migration in the channel, and the
 X. Wan, M. Knoll / Journal of Food Engineering 168 (2016) 79–83 81

conductance between the source and drain can be calculated by The electrical conductance can be integrated as:
the migration length. Therefore, the normalization of the conduc-
d bd d
tance should correspond to the normalization of the migration GðtÞ ¼  r2  Lm ðtÞ þ  r1   r1  Lm ðtÞ ð4Þ
l l l
length. To check the relationship of the conductance and the
migration length, the resistances of the system and migration From Eqs. (1) and (4), we can that the normalized electrical con-
length are recorded simultaneously by a table multimeter and an ductivity is proportional to the normalized the migration length
optical measurement respectively. The comparison of the normal- and square root of time.
izations of the conductance and the migration length is shown in pffiffi
ðDGÞnorm  ðLm Þnorm  t ð5Þ
Fig. 2.
Fig. 2 shows that the changes of normalizations in the migration The conductivity of the pseudo-transistor is changed with the
length and electric conductance fit well. Thus, the resistance migration length. The doping front migration also shows the time
between the source and drain can be modulated easily by the dop- dependency. The migration length is proportional to the square
ing front migration length. The products will not be read out when root of time.
the chemical doping front moves to the end of this two-terminal
device. The resistance of the activation layer increases rapidly 3.2. Temperature dependency in TTI
within a very short time and turn off the system. The change in
resistance for the last 43 h is shown in Fig. 1(b). This phenomenon To evaluate the temperature dependency in the
allows the activation layer to be used as a switch. The switch can pseudo-transistor, the system is activated at different tempera-
turn off the RFID tag quickly at the end of the shelf life of products. tures. The migration coefficient (km) is calculated by Eq. (1). The
The normalizations in the migration length and electric conduc- result is shown in Fig. 3.
tance can be explained as follows. The migration velocity of doping front in the pseudo-transistor
The migration length in the electrochemical pseudo-transistor increases with the rising temperature and shows a temperature
is a function of time (Nolte et al., 2011). dependency. This mechanism can be discussed in two models.
pffiffi When the doping front migration in the transistor is in a diffusion
Lm ðtÞ ¼ km t ð1Þ
model, the migration coefficient is proportional to the diffusion
where Lm(t) is the migration length at time t, and km is the migra- coefficient, which is a function of temperature (Nyström et al.,
tion coefficient. 1981).
The electrical conductance of the pseudo-transistor (see
km  D ð6Þ
Fig. 1(a)) can be written as:
Z b
d b ln km  ln D ¼ a þ ð7Þ
GðtÞ ¼ rðx; tÞdx ð2Þ T
l 0 where a and b are constants; D is the diffusion coefficient; and T is
where r is the electrical conductivity of the activation layer in TTI; the absolute temperature. The diffusion in polymers shows temper-
G(t) is the electrical conductance of the pseudo-transistor at time t; l ature dependence. The diffusion coefficient depends on the
is the width of the doping channel; b is the length of the temperature.
pseudo-transistor; x is the direction of the doping front migration; Another possible model is the capillary model, in which the
and d is the thickness of the activation layer. migration and activation layer are in a capillary between two
The electrical conductance of the activation layer is composed encapsulation films. The total thickness of the layers is the distance
of two parts of the activation layer. When r1 and r2 are the electri- between the parallel plates. The flow distance of the liquid
cal conductivity of the different states of the activation layer, x is between parallel plates is a function of time and distance between
the position of the doping front at time t. the parallel plates (Schwiebert and Leong, 1996).
Z LðtÞ Z b sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
d d
GðtÞ ¼ r1 ðxÞdx þ r2 ðxÞdx ð3Þ pffiffiffiffiffiffiffiffiffi c cos h
l 0 l LðtÞ L ¼ Uht ¼ ht ð8Þ
3g

where L is the flow distance; h is the distance between the parallel

plates; U is the coefficient of planar penetrance; c is the surface ten-
sion of the liquid–vapor interface; h is contact angle; t is time; and g
is the absolute viscosity of the fluid.
The viscosity of fluid also shows temperature dependence
(Fogel’son and Likhachev, 2001) and can be described as:
 
E
g ¼ g0 exp ð9Þ
kðT þ T 0 Þ
where g is the absolute viscosity of the fluid; T is the absolute tem-
perature; T0 is the correction temperature; g0 is the viscosity of the
fluid at T0; E is the energy; and k is a constant.
Deformed Eq. (8)
sffiffiffi rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
1 c cos h pffiffi pffiffi
L¼  h  t ¼ kp t ð10Þ
g 3
Fig. 2. Comparison between the normalized migration length and the normalized
From Eqs. (9) and (10)
conductance (8.5 lm PVA/HEC migration layer on 1.0 lm PANI layer activated in
0.5 M NaOH aqueous. Migration length is 15.8 mm in 128 h. Resistance range: 1.91–
2.36 K X. Temperature: 23 ± 0.5 °C. The activation is not ended and the migration
b1
ln kp ¼ a1 þ ð11Þ
front is still running). T
82 X. Wan, M. Knoll / Journal of Food Engineering 168 (2016) 79–83

Fig. 3. Migration lengths (Lm) at different temperatures in the pseudo-transistor. (a) 8.5 lm PVA/HEC migration layer on 1.0 lm polyaniline layer is activated in 0.5 M NaOH
aqueous. R2 is 0.99, SD in four samples. (b) Natural logarithm of migration coefficient (km) against the reciprocal of the absolute temperature (1000/T), R2 is 0.99.

Both Eqs. (7) and (11) show the temperature dependency of the
distance of the migration in a similar formation. The migration
length is a function of the temperature in these two models. The
experimental data fit the models well.
In these two models, the activation energy of TTI can be calcu-
lated by the natural logarithm on both sides of the Arrhenius
function:
Ea
ln k ¼ þ ln A
RT
where Ea is the activation energy, R is the universal gas constant, T is
the temperature, and A is the pre-exponential factor. The slope
(Ea/R) and the intercept (ln A) were obtained by linear regression.
The Arrhenius activation energy is estimated by Eq. (12) and the
result is 129.61 kJ/mol. This Ea value of this device is closed to the
one with Ea = 103.2–127.3 kJ/mol which was reported by Vaikousi
et al. (2009) and with Ea = 102–114 kJ/mol which was reported by
Yan et al. (2008). The activation energy of TTI in the market is
around 100 kJ/mol. The Ea of TTI from Visab is ranged from
68.7 kJ/mol to 102.1 kJ/mol and Onvu label’s Ea is in the range
92.79–105.75 kJ/mol (Zabala et al., 2015).
Comparing the different TTIs, the activation energy in TTI based
on doping in conductive polymer is little higher than which in
others TTIs with different mechanisms. It can be explained by
the addition of the transport energy in a channel and the reaction
energy in the system. The result shows that the migration length in
this device can be recorded the history of time and temperature.
Given that the migration length, which has time and tempera-
ture dependency, can cumulate the temperature history of the per-
ishable food over time, the pseudo-transistor with performances of
time and temperature dependency could act as an eligible TTI that
provides basic functions, such as clock, temperature sensor, and
electrical switch.
can turn off the circle of RFID tag in last few minutes, the switch
is caused by the migration front moving to end of the channel
(Fig. 4). As the RFID reader cannot read any information from the
sample, the product should not be used any more.
The migration length and resistance of the TTI changing with
the temperatures are shown in Fig. 4. The migration velocity is
response to temperatures in this TTI–RFID system with 1.33 cm
activation layer. The activation in TTI–RFID device is end after
ð12Þ 125 h. Its resistance is ranged from 2.76 K X to 15.47 K X and to
390 K X in last few minutes. The circle of RFID tag is turned off.
The TTI–RFID device can be read by the RFID reader before it
switched off.
To supervise different shelf life of perishable products, the
length of activation layer can be designed easily in different sizes.
It is also possible to change migration layer to control the migra-
tion velocity (Nolte et al., 2011). Normally the TTI–RFID device
can be designed to suit the particular needs of products. For exam-
ple, the migration length or the material of migration layer can be
chosen to dominate the time which decided by the shelf life of dif-
ferent products.
To compare with existing TTIs, this new type TTI is not only cap-
able of indicating the cumulative time–temperature history by the
migration length of the chemical doping front but also capable of

3.3. Switch in TTI–RFID device

Conductivity is necessary to connect the TTI with an RFID tag.

The RFID tag can be connected with the TTI (see Fig. 1(b)) because
the pseudo-transistor-TTI is fabricated by conductive polymer. The
RFID tag can be read by an RFID reader (USB, ISO15693) when the
TTI has low resistance. After TTI–RFID device activates at changing
temperatures, the migration length increases with time and high Fig. 4. Migration lengths (Lm, blue j) and resistances (red ) at different
temperature. But the resistance changes little at first period and temperatures in TTI–RFID system. (For interpretation of the references to color in
greatly at last period. When the transistor acts as a switch which this figure legend, the reader is referred to the web version of this article.)
 X. Wan, M. Knoll / Journal of Food Engineering 168 (2016) 79–83
turning off the RFID tag when the perishable product is exposed to
excessive temperatures. So this TTI–RFID device based on conduc-
tive polymer can offer double supervisions to the safety of perish-
able foods, vaccines and blood products. The reaction in this TTI is
between the conductive polymer and solution, it works well at a
temperature ranged 0–40 °C. But it still should be used carefully
to notice the freezing point of the solution in a cold chain.
4. Conclusion
From the results above, it can be concluded that the migration
length in TTI based on an electrochemical pseudo-transistor with
a chemical doping front in conductive polymers is depended on
time and temperature and the activation energy of TTI is close to
the one can be used as a smart and powerful TTI in the studies
and market. The TTI when combined with the RFID tag can provide
a new alternative strategy to supervise and trace the safety of per-
ishable food by using an intrinsically conductive polymer. Both the
TTI and the RFID reader can avoid the misuse of products which are
exposed to high temperature. Consequently, the TTI–RFID system
can give double protections of the safety of perishable foods.
Acknowledgements
This work is part of the ‘‘Science-to Business PreSeed’’- project
‘‘ElektronischesMindesthaltbarkeitsdatum’’ which is supported by
the state of North Rhine-Westphalia (Germany) and the
European Commission (EFRE). It is also supported partly by the
Research Fund for the Doctor program (11021) of Anhui
University of Science and Technology and sponsored by the
Scientific Research Foundation for the Returned Overseas Chinese
Scholars, State Education Ministry.
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