ECS Transactions, 64 (20) 21-30 (2015)

10.1149/06420.0021ecst ©The Electrochemical Society

Supercapacitors Based on Propylene Carbonate with

Addition of Sulfur Containing Organic Solvents

J. Eskusson, A. Jänes, T. Thomberg, and E. Lust

Institute of Chemistry, University of Tartu, 14a Ravila Street, 50411 Tartu, Estonia

The electrochemical characteristics of electrical double layer

capacitors consisting of the mainly microporous titanium carbide
derived carbon (TiC-CDC) electrodes in 1 M (C2H5)3CH3NBF4
solutions in propylene carbonate (PC) and mixtures of PC with
diethyl sulfite (DES) or 1,3-propylene sulfite, (PS) at different
volume ratios have been studied using cyclic voltammetry,
electrochemical impedance spectroscopy, constant current
charge/discharge and constant power methods. The specific
capacitance, phase angle and other values dependent on the solvent
system used and temperature applied (from -45 ºC to 60 ºC) have
been established. The region of ideal polarizability E ≥ 2.7 V has
been demonstrated for TiC-CDC electrodes in all mixed non-
aqueous electrolytes and at temperatures investigated. Specific
conductivity values have been obtained and correlated with the
electrochemistry data. The limiting capacitance, the characteristic
time constant and complex power and energy values calculated
depend noticeably on the solvent mixture used, i.e., on the specific
conductivity of electrolyte solution.

Introduction

Supercapacitors (SCs) with better performance and longer cycle life are of interest for
electric vehicle producers.Very important problem is associated with the development of
non-aqueous electrolytes and its designed properties obtaining the characteristic
relaxation frequencies, energy and power densities and other important characteristics of
SCs. The energy and power density and coulombic efficiency depend on the region of
ideal polarizability of the interface between the nanoporous carbon electrode and non-
aqueous electrolyte solution (1). The replacement of acetonitrile (AN) with less harmful
and less flammable solvent or mixtures of non-aqueous solvents is a very important step
for the wide commercialization of SCs, because AN is a toxic solvent and cannot widely
used for the production of SCs for the consumer goods and computer back-up systems, as
well as for other various peak power generation systems. One possibility to increase the
conductivity and decrease the viscosity of electrolyte is to use some electrolyte additives
or so-called co-solvents (2,3).
Many studies were performed on the optimization of the lithium-ion battery
electrolytes using solvent mixtures. Most of the alternative electrolyte solutions which are
currently used are composed of non-aqueous solvents (or mixtures of solvents) such as
propylene carbonate (PC), ethylene carbonate (EC), diethyl carbonate (DEC), dimethyl
carbonate (DMC), ethylmethyl carbonate (EMC) for tetraalkyl ammonium cation

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 ECS Transactions, 64 (20) 21-30 (2015)

(generally tetraethylammonium tetrafluoroborate ((C2H5)4NBF4) or

triethylmethylammonium tetrafluoroborate ((C2H5)3CH3NBF4) salts (4).
Cyclic PC and EC have a good compatibility with carbon electrodes, a high dielectric
constant, and enabling the dissolution of salts up to sufficient concentrations. However,
these electrolytes are highly viscous and give poor conductivity even at ambient
temperatures. When PC or EC is mixed with linear alkyl carbonates, such as DEC, DMC
or EMC, more rapid ion transport is achieved as a result a lower viscosity and
subsequently the higher ionic conductivity is observed. The resulting binary or ternary
mixed solvent solutions are widely used in commercially available lithium ion batteries.
It was demonstrated that the choice of co-solvent is a critical issue that significantly
affects not only the conductivity, but also the electrochemical performance, including the
physicochemical properties of solid electrolyte interface (SEI) formation. In recent years,
sulfites such as dimethyl sulfite, glycol sulphite and butylene sulfite have been studied as
a film forming additives for electrolytes in lithium ion batteries and supercapacitors (5,6).
Diethyl sulfite (DES) is used as high temperature additive for carbonate-based
electrolytes in lithium ion batteries. It improves the decomposition resistance of the
electrolyte (7). Propylene sulfite (PS) exhibits promising performance characteristics for
use as a film-forming electrolyte additive in lithium ion batteries (8).
The main aim of this paper was to study the influence of the binary solvent system
characteristics, based on the propylene carbonate mixtures with diethyl sulfite (DES,

Sigma-Aldrich 98 %) in different volume ratios on the microporous TiC-CDC electrode 

Sigma-Aldrich > 99.5 %) or 1,3-propylene sulphite (noted as propylene sulphite, PS,

electrolyte interface characteristics. Some physical characteristics and the molecule

dimensions, calculated using GAUSSIAN 03 software (DFT-B3LYP theory and 6-31G*
basis set) for different solvents used are given in Scheme 1 and Table 1. Noticeable
dependence of parameters on the chemical composition has been established.

Scheme 1. “Space Filled” representations of propylene carbonate, propylene sulfite and

diethyl sulphite and the molecule dimensions (height (h) and width (w)) calculated using
GAUSSIAN 03 software (DFT-B3LYP theory and 6-31G* basis set). Atoms are denoted
as follows: hydrogen - white, carbon - grey, sulfur – yellow and oxygen - red.

In this work the electrochemical characteristics of SCs have been obtained using the
following solvents and solvent systems mixed in the various volume ratios: pure PC,
PC:DES (95:5), PC:DES (90:10), PC:PS (95:5), PC:PS (90:10) and PC:PS (80:20). These

melting temperatures, the relative macroscopic dielectrical permittivity () values (Table
systems have been selected because mentioned solvents have different viscosity and

1), influencing noticeably the double layer characteristics.

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 ECS Transactions, 64 (20) 21-30 (2015)

Table 1. Physical characteristics of different solvents used for studies.

Experimental

All the experiments discussed were made inside the glove box “MBraun Labmaster
sp" at very clean and dry conditions (O2 and H2O concentration lower than 0.1 ppm). The
two-electrode symmetrical system was set in a hermetic aluminium test cell (Hohsen

the 25 m thick Nippon Kodoshi TF4425 separator sheet was used. The pure argon
Corporation, Japan) to ensure the gas tightness of the cell. Between working electrodes

(99.9999 %, AGA) has been used for saturation of the propylene carbonate (“Sigma-
Aldrich”, anhydrous, 99.7 %, moisture content by Karl Ficher titration method less than
20 ppm), diethyl sulphite (“Aldrich”, 98 %, moisture content less than 35 ppm), and
propylene sulphite (“Aldrich”, assay 99.5 %, moisture content less than 30 ppm). All

(C2H5)3CH3NBF4 (Stella Chemifa, assay  99.9 %, moisture content < 100 ppm,
solvents have been stored over molecular sieves before used for preparation of the 1 M

additionally purified and tested) electrolyte. The electrochemical behavior of SCs was
tested applying the cyclic voltammetry (CV), constant current charge/discharge (CC/CD),
electrochemical impedance spectroscopy (EIS) and the constant power (CP) methods.
Impedance spectra were recorded over ac frequency, f, range from 3 × 105 to 1 × 10-3 Hz
with 5 mV modulation, using a 1252A Solartron FRA and SI1287 potentiostat.
Specific surface area, pore size distribution, micropore volume, micropore area and
other parameters were measured using the Micromeritics ASAP 2020 (Micromeritics,
Inc.) system and calculated according to the methods discussed in (2-4,6). The electrodes
were constituted of the porous titanium carbide derived carbon (TiC-CDC powder,
synthesized at T = 950 ºC from TiC powder (Alfa Aesar), mixed with 6 wt % of binder
(polytetrafluoroethylene 60% dispersion in H2O, “Sigma-Aldrich”) and roll-pressed
together to form a flexible electrode layer with thickness 100 ± 5 m. After drying under
vacuum, the electrodes were covered by the very pure Al layer from one side by the
electromagnetron sputtering method. The limits of ideal polarizability of Al layer,
established by cyclic voltammetry as well as by impedance spectroscopy methods, are

the Ti-CDC electrodes were heated at T = 120 C for 48h under reduced pressure. The
wider than for TiC-CDC electrodes used. Before assembling of the symmetrical SC cells,

electrode area used was 2 cm2 (6).

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 ECS Transactions, 64 (20) 21-30 (2015)

Fig. 1. Specific conductivity, solvent composition dependences with addition of 1 M

(C2H5)3CH3NBF4 measured at different temperatures.

Fig. 1 demonstrates dependence of the specific conductivity,  measured at different

temperatures in the mixed solvent system. As it can be seen in Fig. 1,  nearly

electrolyte systems the highest  value has been measured for PC:DES (90:10) solvent
exponentially decreases with the decrease of temperature and for different mixed

system.

capacitance vs. cell potential (C, E), presented in Fig. 2a and b, show that for various
The nearly rectangular shape of the cyclic voltammograms (CV), expressed as

behaviour has been established at cell potential scan rates v  10 mV s-1 and at E  2.7
mixed solvent systems at different temperatures the so-called nearly ideal capacitor

V. This is valid even at T = -20 ºC. The potential scan rate at which the deviation of
cyclic voltammograms from the nearly rectangular shape can be seen in the region of
potential switch over decreases with the decrease of density of the electrolyte.
(a) (b)

Fig. 2. Cyclic voltammograms expressed as capacitance vs. cell potential curves for
PC:PS (95:5) solvent system with addition of 1 M (C2H5)3CH3NBF4 at cell potential scan
rate 10 mV s-1 measured at different temperatures (a) and for different solvent systems
with addition of 1 M (C2H5)3CH3NBF4 at cell potential scan rate 10 mV s-1, measured at
temperature -20 ºC (b).

It should be mentioned that the values of capacitance C can be calculated from j, E curves

C  j (dE / dt ) 1 ,
according to Eq. 1:

if we assume that the capacitance C is constant (C  f(E)) and if the series resistance
[1]

Rs  0 or if the current j  0 (d(E)/dt = v is the potential scan rate). In a symmetrical

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 ECS Transactions, 64 (20) 21-30 (2015)

(two-electrode) system used the specific capacitance Cm (farads per gram) of the
activated carbon can be obtained from the capacitance of the cell by Eq. 2:
Cm 
2C
m , [2]
where m is weight (g) of the one TiC-CDC electrode if, to the first approximation, we

fixed E. Thus, Eq. 1 can be used for obtaining the capacitance values only in the region
assume that the positively and negatively charged electrodes have the same capacitance at

of small potential scan rates if the values of current are very small (as the potential drop
(jR drop) losses are negligible only at these conditions) and the current response is
essential of a pure capacitor.
Data measured at different temperatures (Fig. 2a) indicate that only at T ≥ 60 ºC,

and at E > 2.3 V, some faradaic processes started. With the decrease of temperature
some deviation of system from ideally polarisable system behaviour has been established,

lower than 0 ºC, a noticeable decrease of capacitance takes place. However, even at -45
ºC remarkable capacitance values (Cm  60 F g-1) have been detected. Analysis of the
experimental data demonstrates that there is noticeable dependency on solvent mixture

and PC:PS (80:20) electrolytes, the values of Cm are practically independent of v, if v 

used (Fig. 4a). For PC, PC:DES (95:5), PC:DES (90:10), PC:PS (95:5), PC:PS (90:10)

10 mV s-1 (Fig. 2b).

For more detailed analysis of SCs the complex impedance (so-called Nyquist) plots
have been measured and analysed. According to the Nyquist plots (Z’ is the real part of
impedance and Z” = (jCs)-1 is the imaginary part of impedance (angular frequency  =
2f), given in Figs. 3a and b, for PC, PC:DES (95:5), PC:DES (90:10), PC:PS (95:5),
PC:PS (90:10) and PC:PS (80:20) electrolytes studied, the fairly conventional behaviour
for a two porous electrode system with uniformly distributed solution series resistance Rs
and double layer series capacitance Cs is exhibited.

Fig. 3. Nyquist plots at cell potential E = 2.7 V for the SCs, based on different solvent
systems at T = 20 ºC (a) and for solvent system PC:PS (90:10) at different temperatures
(b) with addition of 1 M (C2H5)3CH3NBF4.

Only for PC:DES (95:5 and 90:10) solvent mixtures based supercapacitors, some
deviations have been seen. At T = 60 ºC, noticeable deviations from ideally polarizable
interface has been established (Fig. 3b). Very strong influence of high frequency series
resistance on the Nyquist plots shape has been observed at T ≤ -35 ºC. Extrapolation of
the high frequency part of the Z”, Z’ curve to the condition Z” = 0 gives the so-called
equivalent series resistance of the cell (ESR) (RE = Z’() = Rs()). RE values
depend on the solvent or mixed solvent system used and RE decreases in the order: PC:PS
(95:5) > PC > PC:PS (90:10) > PC:PS (80:20) PC:DES (95:5) < PC:DES (90:10).

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 ECS Transactions, 64 (20) 21-30 (2015)

(a) (b)

Fig. 4. Cs vs. ac frequency plots at cell potential E = 2.7 V for the SCs, based on
different solvent systems at T = 20 ºC (a) and for the PC:PS (90:10) solvent system based
supercapacitor at different temperatures (b) with addition of 1 M (C2H5)3CH3NBF4.

Similarly to the other non-aqueous electrolyte systems, noticeable increase of Cs (Fig. 4a)
at f > 1.0 Hz takes place, and at f > 310-2 Hz, well expressed plateaus in Cs, log f -plots

systems. At f = 310-2 Hz, the low frequency Cs (0) values increase from PC:DES
have been established, except for PC:DES (95:5) and PC:DES (90:10) mixed solvent

(90:10) to PC:PS (95:5) mixed solvent system. The Cs values depend very strongly on the
temperature applied, given in Fig. 4b.
CV measured at 10 mV s-1 and at 60 ºC shows a reversible capacity about 100 F g-1
similar to that measured at 20 ºC (Fig. 2). At the same time, capacitance obtained from
low-impedance branch (Fig. 4b) remains at the same level (105 F g-1) for 20 ºC and 0 ºC,
but is about 6 times less for 60 ºC. It seems that the stationary state was easily reached for
temperatures equal or lower 20 ºC rather than for 60 ºC. It should be noted that CV
measured at 10 mV s-1 (i.e. relatively quickly) is affected to much less extent by the
parasitic reactions than data measured by impedance method taking significantly longer
time during which very low concentration contaminants can adsorb at TiC-CDC
electrode and thereafter participating in some faradic reactions and thus blocking the
active surface area of supercapacitor electrodes. Similar surface blocking effect for
reaction intermediates or products has been observed for EMImBF4|TiC-CDC interface at
100 ºC (9).
The values of the real and imaginary part of capacitance have been calculated

C ()  C ' ()  jC" () ,

according to Eqs. 3 and 4:

Z " ( ) Z ' ( )
[3]
C ' ( )   C" ( ) 
 Z ( )  Z ( )
2 2

where Z() is the complex impedance. It should be mentioned that the low frequency part
, , [4]

of C’ for the supercapacitor cell corresponds to the so-called static capacitance, which is
measured during the constant current discharge/charge steps, and C” corresponds to the
energy dissipation of the capacitance Cs(), i.e., it corresponds to the energy dissipation
by an irreversible processes, which can lead to the hysteresis of the electrochemical
processes (10).

called relaxation frequency, fR, determining the characteristic time constant R1 = (2fR)-1
According to the results in Fig. 5, the C”, f- dependencies have a maximum at the so-

(Fig. 5, inset). R1 depends noticeably on the solvent system used and R1 increases with
the decrease of the specific conductivity of the electrolyte. With the decrease of T, R1

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 ECS Transactions, 64 (20) 21-30 (2015)

increases noticeably, and at T < -20 C, the R1 value cannot be calculated for PC:PS

For other systems more pronounced dependence of R1 on T has been observed. Analysis
(95:5) mixed solvent system electrolyte due to the absence of maximum in C", log f -plot.

R1. It can be seen in Fig. 5 inset, that for PC:PS (95:5) mixed solvent system, R1 is
of the data in Fig. 5 shows, that only half of the low-frequency capacitance is reached at

lowest for temperatures from -20 to 20 ºC.

Fig. 5. Imaginary capacitance C” vs. ac frequency plots at cell potential E = 2.7 V for

(C2H5)3CH3NBF4 measured at different temperatures. Inset: relaxation time constant R1

the PC:PS (95:5) solvent system based supercapacitors with addition of 1 M

vs. temperature plots for different solvent systems at different temperatures.

S ( )  P( )  jQ( ) ,
The values of complex power can be expressed as (10)
[5]
where the real part of power is expressed as
P( )  C" ( ) Erms
2

[6]
and the imaginary part of power as
Q( )  C ' ( ) Erms
2

, [7]
Erms  Emax 2
2

with (Emax is the maximal amplitude of ac potential). Ideal capacitor

(a system with the ideal capacitive behaviour) has no real part as there is only the reactive

jE rms
contribution to the complex power. Hence Eq. 5 simplifies to:
S ( )  jQ     jCE rms
2
2

Z"
. [8]
Systems with the ideal resistive behaviour have no imaginary part as this component only

E rms
dissipates energy and the complex power takes the well-known form:
S ( ) 
2

Z'
. [9]

resistive at high frequencies (  ) and capacitive at low frequencies (   0).

It should be noted that real supercapacitors balance between two states mentioned before:

transmission like circuit (11-14). The dependence of the normalised real part (P()/|S|)
Between these two states supercapacitor behaves like a resistance-capacitance (RC)

and imaginary part (Q()/|S|) for the complex power on ac frequency are presented in Fig.

the frequency of the intersection point of the (P()/|S|), logf- and (Q()/|S|), logf- plots
6. In a good agreement with the data in Fig. 6, the relaxation time constants, obtained as

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 ECS Transactions, 64 (20) 21-30 (2015)

(R2 = (2fR)-1) (Fig. 6, inset), are very different for cells filled with PC, PC:PS (95:5),
PC:PS (90:10) and PC:PS (80:20) compared with PC:DES (95:5) and PC:DES (90:10)
electrolytes. Thus, comparison of the data for the cells filled with various solution
systems indicate the huge influence of the molar conductivity (Fig. 1) of the solvent at
moderate and low ac frequencies on the limiting capacitance and time constant values.

noticeable dependence of R2 on T and R2 values obtained at T = -35 ºC are nearly 1.5 - 2
Data in Fig. 6 (inset) show, that for PC:DES (95:5) and PC:DES (90:10), there is a

times longer than R2 obtained at 60 ºC.

Fig. 6. Normalized reactive power Q/S and active power P/S vs. ac frequency plots at
cell potential E = 2.7 V for the SCs, based on the PC:PS (95:5) solvent system with

constant R2 vs. temperature plots for different solvent systems at different temperatures.
addition of 1 M (C2H5)3CH3NBF4 at different temperatures. Inset: relaxation time

density (Emax) and power density (Pmax) values at E = 2.7 V were calculated (Fig. 7)
For better comparison with our previous studies, the maximum theoretical energy

Cs Sel E 2
according to Eqs. 10 and 11:
Emax 
2 m 3.6 ,
E 2 Sel
[10]
Pmax 
4 RE m . [11]

Fig. 7. The maximum specific energy (Emax) vs. specific power (Pmax) plots at E = 2.7 V
for the SCs, based on different solvent systems at T = 20 ºC.

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 ECS Transactions, 64 (20) 21-30 (2015)

In Eqs. 10 and 11 Cs (F cm-2) is the series capacitance at f = 110-3 Hz, Sel is the flat
cross-section surface area of electrodes (2.0 cm2), m is the mass of two electrodes (g), RE
(Ω cm2) is the high-frequency series resistance and 3.6 comes from conversion of time
and mass units. Data in Fig. 7 show that Emax is practically independent for all solvent
systems studied (25 – 30 W h kg-1). However, there is very noticeable dependence of Pmax
on solvent system used and the highest value of Pmax calculated for PC:PS (95:5) solvent
mixture is caused by the higher Cs and lower Rs values.
Constant power discharge tests have been conducted using two electrode SCs at
different temperatures. The energy and power relationships, so-called Ragone plots
(taking into account of the total active material weight of two electrodes) for the
supercapacitors based on the TiC–CDC electrodes at different temperatures have been
calculated within the cell potential range from 2.7 V to 1.35 V. The results calculated
based on the optimal power density values (10-s and 2-s power) are given in Figs. 8a and
b. It can be seen that quite high energy density (~ 25 - 27 W h kg-1) values at moderate
power densities (~ 1 kW kg-1) have been measured for PC:PS (95:5) mixed system. Data
in Fig. 8a show that at - 20 ºC, the specific energy and specific power are strongly
dependent on the composition of mixed solvent system, caused by different values of Cs
and Rs calculated.

Fig. 8. Ragone plots for the SCs completed using TiC-CDC electrodes in 1 M
(C2H5)3CH3NBF4 on different solvent systems at temperature -20 ºC (a), and for the SCs,
based on PC:PS (95:5) solvent system at different temperatures (b), obtained from
constant power tests within the cell potential range from 2.7 V to 1.35 V.

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 ECS Transactions, 64 (20) 21-30 (2015)

Conclusions

The electrochemical characteristics of the supercapacitors consisting of the mainly

microporous titanium carbide derived carbon (TiC-CDC) electrode in 1 M
(C2H5)3CH3NBF4 solutions in propylene carbonate (PC) and mixtures of PC with diethyl
sulfite (DES), and 1,3-propylene sulfite, (PS) at different volume ratios of DEC:PC or
PS:PC, have been obtained using the cyclic voltammetry, electrochemical impedance
spectroscopy, constant current charging/discharging and the constant power methods.
The specific capacitance, phase angle and other values dependent on the solvent system
used and temperature applied (from -45 ºC to 60 ºC) have been established. The region of
ideal polarizability E ≥ 2.7 V has been demonstrated for TiC-CDC electrodes in all
mixed electrolytes and at temperatures investigated. Ragone plots (measured taking into
account of the total active material weight of two electrodes) for the supercapacitors
show that quite high energy density (~ 25 - 27 W h kg-1) values at moderate power
densities (~ 1 kW kg-1) have been established for PC:PS (95:5) mixed system at T ≥ -20
ºC. However, the specific energy and specific power values are strongly influenced by the
composition of mixed solvent system, caused by different values of Cs and Rs calculated
for supercapacitor systems.

Acknowledgements

The present study was supported by The Estonian Centers of Excellence in Science: High
Technology Materials for Sustainable Development, ETF Project 9184, European
Regional Development Fund Project SLOKT10209 T and institutional research funding
IUT20-13 of the Estonian Ministry of Education and Research.

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