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A R T I C L E I N F O A B S T R A C T
Keywords: In this work, thermally stimulated spectroscopy methods are applied to PET films to analyse the electret state.
Track membrane The thermally stimulated discharge currents, or thermally stimulated depolarization of track-etched like mem
Polyethylene terephthalate brane samples obtained at different technological stages of their manufacture, have been investigated. The
Swift ions
analysis of thermally stimulated depolarization currents indicates a significant change in the spectra of energy
Electrets
Thermal activation
states of the electric charge accumulated during PET films’ polarization after irradiation with accelerated swift
Thermally stimulated current Xe ions, ultraviolet treatment, and alkaline etching of the latent tracks. The Eyring method was used to calculate
the parameters of the relaxation processes occurring in irradiated PET, such as the activation energy and the
effective frequency factor. The significant change in the spectra of energy states of the electric charge accu
mulated during polarization in PET films due to ion-track processes indicates the possibility of creating an
electret state in irradiated PET films and track membranes.
* Corresponding author. Joint Institute for Nuclear Research, 6 Joliot-Curie St., Dubna, Moscow, 141980, Russia.
E-mail address: rossouw@jinr.ru (A. Rossouw).
https://doi.org/10.1016/j.radphyschem.2021.109868
Received 27 May 2021; Received in revised form 9 September 2021; Accepted 5 November 2021
Available online 9 November 2021
0969-806X/© 2021 Elsevier Ltd. All rights reserved.
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
the medium locally along the particle’s trajectory, leading to the exci Table 1
tation and ionization of atoms. The energy released along the trajectory List of samples, etching time and average surface pore diameter of irradiated and
of a swift ion leads to the formation of a continuous extended structural alkaline treated PET film.
defect called a track. As a rule, xenon and krypton ions with a large Sample Etching Average SEM surface pore Additional comments
specific energy loss (MeV /μm) are used to form latent tracks in PET. As a Number time (min) diameter, ±10% error, (SEM cross-section
result of irradiation with swift ions, amorphization of PET and a (nm) view)
decrease in the size of crystallites is observed (Blonskaya et al., 2021). 1 0.5 25 Partially etched
Additionally, PET macromolecules’ destruction is accompanied by an 2 1 36 Partially etched
3 2 57 Partially etched
increase in the number of carboxyl groups in the polymer (Apel et al.,
4 3 78 Partially etched
1999; Tuleushev et al., 2020). 5 4 160 Fully etched
Tracks in PET are capable of selective chemical etching when 6 6 232 Fully etched
exposed to aqueous solutions of alkali metals. In ester polymers, 7 – – Original film
including polyethylene terephthalate, a chemical reaction of the etchant 8 – – Original film + UV
interacts with the breaking of ester bonds, the elimination of ethylene *Note, cross-sectional pore diameter has not been indicated as only correlation
glycol and terephthalate ion molecules with the formation of carboxyl between TSD and film surface /surface pores were investigated.
and hydroxyl groups on the surface, which determine the negative
electric charge of the surface of the material in contact with aqueous of the charged surface of irradiated PET films and track-etched mem
media. In order to increase the selectivity of track etching, the method of branes based on polyesters is required to expand the spectrum of their
photooxidation of radiolysis products in tracks under the action of "soft" practical application. Incorporating electret properties into these ma
ultraviolet (UV) radiation in the presence of oxygen is used (Apel, 2001; terials could lead to further application in packaging materials for the
Ditlov et al., 1997; Enge, 1995; Fink, 2004; Kaniukov et al., 2017). food industry, filters and membranes, biomedical technology and con
It should be noted that PET films are also used to produce electrets verters such as in hydrogen production.
with a steady electrical charge. An electret is a dielectric that retains a
polarized state for a long time after removing the external influence, 2. Materials and methods
which leads to the polarization (or charging) of this dielectric and cre
ates a quasi-constant electric field in the surrounding space. The electret 2.1. Sample preparation
state, one way or another, is inherent in all dielectrics, including PET
(Brzeziński et al., 2009; Cañadas et al., 2019; Gasanov et al., 2012; Similar to the method used in track-etched membrane production,
Kravets et al., 2013; Lacabanne et al., 1979; Schneider and Wendorff, samples were made from Hostaphan RNK PET film, 30 μm thick, man
1984). ufactured by Mitsubishi Polyester Films. According to the manufacturer,
Analysis of the literature has shown that the methods of ion-track the film is produced by co-extrusion from a melt and consists of an inner
electreting of polymer films are not described in the literature. It can layer free from filler particles and thin outer layers of polymer con
be assumed that, by analogy with the types of electrets presented above, taining a small additive of nano-dispersed silicon dioxide. The film is
the electret properties of a polymer film will change as a result of subjected to biaxial drawing and subsequent heat treatment during
bombardment with accelerated swift ions and under the influence of UV production, which forms a semi-crystalline polymer structure. The
irradiation and alkaline etching of tracks. This will be associated with a density of the film material is 1.4 g /cm3. Irradiation with 132Xe + 26 ions
change in the PET film’s morphology and chemical structure after was carried out by a beam with an energy of 1.16 MeV/nucleon at an
exposure to both ionizing radiation and highly alkaline thermal angle of ± 35◦ sequentially from both sides on the IC-100 cyclotron at
hydrolysis. the FLNR JINR. The ion penetration depth in PET was about 20 μm. The
The thermo-stimulated depolarization method was applied to anal fluence of ions on each side was N = 4.5⋅108 cm-2.
yse the effect of the ion-track processing of PET on the change in electret The choice of conditions for double-sided irradiation of PET films
properties, we decided to use. Thermal activation spectroscopy is widely with swift ions is due to an assumption that the analysis of the TSD
used to study electrical relaxation processes and, in particular, the would reveal the moment of the formation of through pores in the TM
electret state in various dielectric materials (Bräunlich, 1979; Gor samples. The path length of Xe ions, in accordance with the above-
okhovatsky et al., 1998; Temnov et al., 2013; Turnhout, 1971). One of described irradiation conditions, is of the order of 20 μm. The zone of
the most popular thermo-activation spectroscopy methods used to study intersection of latent tracks is in the range from 5 to 10 μm. Additionally,
charge relaxation in electrets is the method of thermally stimulated film treatment by swift ion irradiation can be used for increasing the
discharge current, or thermally stimulated depolarization (TSD). In this active surface of TMs. Table 1 shows the applied conditions for sample
case, the measurement of thermally stimulated currents is carried out in preparation.
the mode of short circuit of the external circuit (i.e., the external Before etching, all samples were exposed to UV irradiation for 2 h on
measuring circuit’s resistance is much less than the resistance of the each side. Samples of ion-irradiated films were exposed to UV radiation
investigated dielectric). By analysing the shape of the TSD curve (the from LE-30 lamps (Lisma, Saransk, Russia) in air. The intensities
temperature dependence of the initial section of the current peak, the measured with a TPK-PKM radiometer were ~4.03 W /m2 in the UV-A
temperature position of the current maximum, etc.), it is possible to range (315–400 nm) and ~5.09 W /m2 in the UV-B range (280–315
determine from the experimental data the most probable activation nm) and ~479 mW /m2 in the UV-C range (100–280 nm). The chemical
energy of electrically active defects and their effective frequency factor etching was carried out in a thermostat at 80 ◦ C with a NaOH solution
(the methods of processing TSD data are described in detail in (Ditlov concentration of 1 mol /L for various times: between 1 and 6 min.
et al., 1997)). The density of nano- and micropores on the surface was calculated
Thus, in studies on the effect of a corona discharge on PET (Brze using a Hitachi SU8020 scanning electron microscope (SEM). A polymer
ziński et al., 2009; Kochervinskii et al., 1995; Kravets et al., 2013), the matrix’s technique of fragility by mild photooxidation was used to
observed TSD spectra in PET confirmed the presence of both dipole and obtain membrane chips, and the images thereof were studied.
the charge’s spatial relaxation. A two-dimensional analysis of the space The Hagen Poiseuille equation (Hernández et al., 1996; Siddiqui
charge peak in the TSD spectra of PET showed that the influence of the et al., 2016), was used to describe the relationship between pressure,
activation volume might be relevant in determining the space load’s fluidic resistance and flow rate, so as to determine if the irradiated and
behaviour, taking into account the samples’ thermal history. alkaline etched PET films had pores in the form of capillaries or not.
It should be noted that an understanding of changes in the properties
2
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
Fig. 1. Sample 1, etching time 30 s and an average surface pore diameter of Fig. 3. Sample 6, etching time 6 min and an average surface pore diameter of
25 nm. 232 nm.
2.2. Measuring device for thermally stimulated depolarization currents state of track-etched membranes.
3
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
∫ωm ∫Em
j(T) ∼ dω G (E, ω)ξ (E, ω, T, β ) dE (1)
0 0
Fig. 6. TSD curves of the initial polyethylene terephthalate films (1), irradiated with Xe ions (2) and subsequent exposed to UV irradiation (3) at a heating rate of
7 ◦ C /min.
4
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
Fig. 7. Sample 2, TSD curves of polyethylene terephthalate films irradiated with Xe and UV radiation at a time of chemical etching t = 1 min at two different heating
rates: (1) 7 ◦ C /min, (2) 9 ◦ C/min.
Fig. 8. Sample 3, TSD curves of polyethylene terephthalate films irradiated with Xe ions and UV radiation with a chemical etching time t = 2 min at two different
heating rates:: (1) 7 ◦ C /min, (2) 9 ◦ C/min.
during the etching process. effective frequency factor were calculated for all used etching times
As shown from the above Figs. 7–12, the maximum of the peak of the (Table 2).
TSD currents shifts with increasing etching time to the high-temperature As is known (Apel et al., 1997), an increase in the etching time leads
region, and its intensity remains approximately the same. To analyse the to an increase in the pores’ average diameter formed in track mem
experimental data, we used an empirical analysis method based on the branes. Table 2 shows the dependence of the average surface pore
Eyring equation of activated states (2), which usually gives more diameter on the etching time.
physically realistic parameters (activation energy and effective fre It can be noted that the dependence of the activation energy on the
quency factor) of electrically active defects, at least in the case of a low average surface pore diameter is almost linear (Fig. 13), and the effec
temperature of noncooperative relaxation (Eyring and Gibbs, 1951): tive frequency factor has a pronounced nonlinear character (Fig. 14). A
( ) ( ) sharp increase in the frequency factor after 150 nm may most likely
kT ΔH ΔS
ω= exp − exp (2) indicate the formation of through pores in PET films with a sufficient
h kT k
etching time and an increase in the polymer’s free volume. An increase
in the activation energy suggests the formation of deeper and deeper
where k is the Boltzmann’s constant, h is Planck’s constant, ΔH is
traps of charge carriers with an increase in the etching time.
enthalpy and ΔS is entropy.
Using the method of relaxation maps (Doulut et al., 1998), the degree
The relaxation process parameters, the activation energy and the
5
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
Fig. 9. Sample 4, TSD curves of polyethylene terephthalate films irradiated with Xe ions and UV radiation at a chemical etching time t = 3 min at two different
heating rates: (1) 7 ◦ C /min, (2) 9 ◦ C/min.
Fig. 10. Sample 5, TSD curves of polyethylene terephthalate films irradiated with Xe ions and UV radiation at a chemical etching time t = 4 min at two different
heating rates: (1) 7 ◦ C /min, (2) 9 ◦ C/min.
of disorder of the polymer system was calculated. With an increase in the thermal treatment in water for 2 h at a temperature of 80 degrees
etching time, it increases from 25.2 (for an etching time of 1 min) to 36.6 Celsius. Although water undoubtedly affects the spectra, but only by the
(for an etching time of 5 min) and can be a characteristic of the total height of the TSD peak, and not by the position, which indicates the
volume of "loose" polymer along the pore walls, which forms during possibility of PET amorphization both when it is irradiated with swift
etching. ions and when plasticized with water molecules. . Such a treatment can
An additional experiment was carried out on the effect of thermal lead to weak hydrolysis of irradiated PET and its swelling; such changes
treatment of irradiated PET films in water on TSD. Fig. 15 shows the in the spectra as during etching are not observed.
results for irradiated and non-irradiated PET films that have undergone
6
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
Fig. 11. Sample 6, TSD curves of polyethylene terephthalate films irradiated with Xe ions and UV radiation at a time of chemical etching t = 6 min at two different
heating rates: (1) 7 ◦ C /min, (2) 9 ◦ C/min.
etching of tracks in PET film, have a significant effect on the TSD current
spectra. The values of the parameters of relaxers and the degree of dis
order of the polymer system for track-etched like membranes with
different pore diameters were calculated. For the initial PET films,
several relaxation processes are clearly observed, which, as a rule, are
associated with various molecular movements inside the polymer: a
high-temperature process (dipole-segmental) in the temperature range
of 90 ◦ C is associated with orientational rotations of the polar units of
the macromolecule under conditions when segmental movement is
possible Irradiation of PET films with Xe ions and UV radiation signifi
cantly increase the intensity of α-relaxation, which means an increase in
the segmental mobility in the irradiated samples. Further etching of the
films with an increase in the etching time significantly changed the
spectrum of TSD currents both in temperature position and in intensity.
It can be assumed that, in this case, another process takes priority for the
Fig. 12. Sample 2–6, TSD curves of polyethylene terephthalate films irradiated
relaxation of the charge, most likely associated with the formation and
with Xe ions and UV radiation at a heating rate of 7 K /min and a chemical
etching time of 1 - 1 min; 2 - 2 min; 3 - 3 min; 4 - 4 min; 5–6 min.
further emptying of charge traps on the track walls. The maximum of the
peak of the TSD currents shifts with increasing etching time to the high-
temperature region, and its intensity and the dependence of the acti
Table 2 vation energy on the average surface pore diameter are almost linear.
Parameters of the relaxation process observed in etched PET films at different The dependence of the efficiency of the frequency factor has a pro
etching times. nounced nonlinear character. A sharp increase in the frequency factor,
Sample Etching Average surface Activation Effective
most likely, may indicate the formation of through pores in PET films at
number time, min pore diameter energy, eV frequency a sufficient etching time. An increase in the activation energy suggests
(nm) factor, s-1 the formation of deeper and deeper charge carrier traps with an increase
2 1 36 0,70 2,4⋅1010 in the etching time. The results may indicate a significant change in the
3 2 57 0,73 4,4⋅1010 spectrum of energy states of the electric charge accumulated during such
4 3 78 0,76 5,4⋅1010 films’ polarization and the possibility of creating an electret state in such
5 4 160 0,88 1,5⋅1012 materials. The parameters of the relaxation processes of track-etched
6 6 232 0,97 1,1⋅1013
like membranes can be set in accordance with the structural features
of such objects. In conclusion, it can be noted that the TSD method can
4. Conclusions be an effective tool for the analysis of physicochemical changes in
polymer films irradiated with swift ions. The method also makes it
Thermal activation spectroscopy was applied for the first time to PET possible to evaluate the changes occurring in latent tracks because of
films irradiated by swift Xe ions from both sides and then treated with their chemical etching. The possibility of creating an electret state in
alkaline hydrolysis. It is shown that the processes of ion-track technol irradiated PET films by swift ions based on polyethylene terephthalate
ogy, such as irradiation with swift ions 132Xe+ 26, UV sensitization and makes it possible to expand the possibilities of their use as protective
7
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
Fig. 13. Dependence of the activation energy on the average surface pore diameter.
Fig. 14. Dependence of the effective frequency factor on the average surface
pore diameter.
Funding
Permeability Investigation. Natalia Shabanova: Formal analysis, Inves
tigation. Tamara Mamonova: Track-etched membrane preparation.
This work was funded by the National Research Foundation and the
Nikolay Lizunov: SEM and TEM Investigation. Willem Perold: Supervi
Department of Science and Innovation of South Africa (grant number
sion. Alexander Nechaev: Conceptualization, Supervision, Funding
129274) in association with the Joint Institute for Nuclear Research,
acquisition, Writing - Reviewing. All authors discussed the results and
Russia. The research was supported by the Ministry of Science and
contributed to the final manuscript.
Higher Education of the Russian Federation (Project No. FSZN-2020-
0026).
Declaration of competing interest
CRediT author statement The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
Arnoux Rossouw and Dmitry Temnov share co-first authorship. the work reported in this paper.
Dmitry Temnov: Validation, Formal analysis, Investigation, Writing -
Original Draft. Arnoux Rossouw: Conceptualization; Data curation,
Investigation, Writing - Reviewing and Editing. Iliya Vinogradov:
8
D. Temnov et al. Radiation Physics and Chemistry 191 (2022) 109868
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