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

batteries using electrochemical impedance spectroscopy

Petr Vyroubal* , Tomáš Kazda

Department of Electrical and Electronic Technology, Faculty of Electrical Engineering and Communication, Technická 10, 616 00 Brno, Czech Republic

A R T I C L E I N F O A B S T R A C T

Article history:

Received 1 September 2017 Numerical modelling is the method by virtually testing and verifying the functionality of a speciﬁc

Received in revised form 4 October 2017 product or component. The primary goal is to get approximate results of how the system behaves in a

Accepted 11 October 2017 given time and environment. We are able to accept a certain numerical error from a real experiment, thus

Available online 8 November 2017 signiﬁcantly speeding up part of the development of the device. In the ﬁeld of electrochemistry of

lithium-ion accumulators, several variants of numerical models have been proposed that yield

satisfactory results in modelling certain physical ﬁelds of these batteries (electric ﬁeld, temperature ﬁeld,

current ﬁeld).

© 2017 Elsevier Ltd. All rights reserved.

One model is the battery model with its equivalent circuit, frequency with offset of a certain value of the polarization voltage

which is represented by passive components, namely a resistor and (mostly between 1 and 10 mV) [2].

a capacitor. This is a model that describes the internal behaviour of

a battery by RC circuit. However, the problem is to ﬁnd or measure 2. EIS basics

these parameters. One way to get the parameters of this spare

circuit is by means of electrochemical impedance spectroscopy The impedance value of the system is calculated using the ratio

(EIS). of alternating voltage and alternating current. This is composed of

This article deals with the application this method to obtain the amplitude and phase shift values that are dependent on the set

parameters of the equivalent battery circuit and comparing the frequency. Thanks to this, the dependence of the system

charging and discharging curves of a speciﬁc battery with the ECM impedance on the frequency is obtained. The individual chemical

model. elements that make up the measured system differ from each other

by the time constant of the polarization, which causes the

1. Introduction individual components of the impedance to vary with frequency

variations [3] and [4].

00

Electrochemical Impedance Spectroscopy (EIS) allows the These components are: Z0 which is the real impedance, jZ the

observation of the electrochemical and physical processes occur- imaginary impedance and |Z| the total impedance. The ratio of

ring in the monitored system. This is a very sensitive method in impedances "Z0 /Z00 / Z is called the loss factor tgd. EIS requires stable

which the interpretation of results is rather complex due to its high system, which is difﬁcult in practice due to the possibility of

sensitivity. The total measurement result consists of a mixture of inﬂuencing the measurement by external noise, the temperature

responses from all the events that occur in the measured system, change and contamination. It is necessary to perform the

which often leads to ambiguity of the result [1]. measurement in the moment when the electrochemical response

For a good interpretation of the results, it is necessary to of the system is stable. The impedance is described by the formula

understand the physical and chemical essence of the measured according to [5–7]:

system. Then compare the results with other analytical methods, 00

both electrochemical and physical. The basic principle of this Z ¼ Z0 þ jZ ð1Þ

method is to set up a small sinusoidal AC voltage of a given Alternatively, using polar coordinates:

E-mail address: vyroubal@feec.vutbr.cz (P. Vyroubal). electrochemical process with the help of spare electrical circuits.

https://doi.org/10.1016/j.est.2017.10.019

2352-152X/© 2017 Elsevier Ltd. All rights reserved.

24 P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31

which can be connected serial, parallel or mixed. These type are

resistor R, capacitor C and several others. In these circuits, the

capacitor with polarization processes and a resistor with

conductivity of the sample are related.

2.1. Resistor R

so-called Nyquist graph, only by the real axis shift (see Fig. 1). This

shift corresponds to the value of the real resistance. The real

resistance may by dependent on the conductivity of used

Fig. 2. Nyquist graph for capacitor.

electrolyte. The overall impedance of the model represented by

the resistance is:

Z¼R ð3Þ

2.2. Capacitor C

phase change is 90 (see Fig. 2). This is an element that appears in

the Nyquist graph in the negative values of the imaginary axis as a

half-line. With an increasing frequency, the value decreases

towards zero at an inﬁnite frequency. The capacitor corresponds

to two layers at the electrode-electrolyte interface and its capacity

is inversely proportional to the thickness of this double layer. The

overall impedance of the model represented by the capacitor is: Fig. 3. Nyquist graph for inductor.

1

Z¼ ð4Þ

jvC

2.3. Inductor L

changes phase, but unlike capacity + 90 (see Fig. 3). This element,

like the capacitor, will appear in the Nyquist graph as a half-line,

but in the positive values of the imaginary axis. Inductive

behaviour may be due to a different current distribution and a

potentiostatic error, indicating an error in the EIS measurement.

The total impedance of the model represented by the inductor is:

Fig. 4. Nyquist graph for CPE.

Z ¼ jvL ð5Þ

information on the surface structure. The overall impedance of

2.4. Constant phase element (CPE) the CPE model is therefore:

1

It is an element that is similar to a capacitor but, unlike it, the ¼ Y ¼ Q 0 ðjvÞn ð6Þ

Z

phase is changed at a different angle than 90 (see Fig. 4). In the

Nyquist chart, it is again represented as a semi-line which forms where Q is numerically equal to admittance at v = 1 rad/s refers to

the angle a with the real axis. As with a capacitor with increasing the unit [S sn ], n is the slope of the semi-line from 0 to 1. For n = 1 it

frequency, the value decreases towards zero at inﬁnite frequency. is a capacitor and for n = 0 it is a resistor.

CPE therefore behaves as a non-ideal capacity, it provides

2.5. Warburg W

angle a in the Nyquist chart is equal to 45 (see Fig. 5). This element

is used to model the diffusion of ions. It consists of frequency-

dependent CW capacity and RW resistance in a serial combination.

The total impedance of model W corresponds to CPE when n = 0.5:

1

¼ Y ¼ Q 0 ðjvÞ0:5 ð7Þ

Z

A simpliﬁed overview of the processes taking place in the

lithium-ion battery captured by EIS is shown in Fig. 6. These

storages are divided into three parts according to the speed at

which they proceed. Each part is assigned a corresponding portion

Fig. 1. Nyquist graph for resistor. of the progress in the Nyquist chart [8] and [9].

P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31 25

Li-ion mass transfer phenomena which occur in lithium ion battery electrodes and

their respective Nyquist plots (Fig. 6).

lower frequencies, the impedance becomes purely capacitive,

because the lithium ions can no longer diffuse into the material and

Fig. 5. Nyquist graph for Warburg.

the capacity is thus formed by the ions surrounding the electrode

material [13].

The ﬁrst action that occurs (see Fig. 6) is the diffusion within the

electrolyte. The frequency at which this happening is greater than

3. Mathematical physical model

105 Hz, which implies that this action is very fast and takes place in

the order of microseconds. In the Nyquist chart, this plot is simply

We are used the MSMD model (Multi-Scale Multi-Domain),

displayed as a displacement along the axis-x, which implies that it

which comprises for each layer different physical properties.

has no capacitive part and the impedance is pure resistance. This

MSMD model is fully implemented in ANSYS Fluent battery

resistance is then represented in the model by the R1 resistance

module. This MSMD model simulate the electrochemical behav-

(see Fig. 7 below). The value of this resistance corresponds to the

iour at the particle, electrode, and cell domains, with appropriate

distance of the ﬁrst half-circle point from the y-axis [10].

coupling between the scales [10], [11] and [12]. This allows us

The charge transfer between the electrolyte and the electrode is

multiple cell design tested. We are able to simulate the

represented in the Nyquist graph by a semicircle. This part

temperature ﬁeld in 3D, thermal and electrical ﬁelds, which are

corresponds to the parallel combination of R2 and C1 [11]. The

calculated in the active core the battery according to the following

charge transfer occurs approximately in the frequency range of 100

differential equations:

to 106 Hz. This process is slower and takes place in the time range of

10 ms to 1 s. The distance between the ﬁrst and the last point of the @rC p T

semicircle corresponds to the diffusion occurring in the electrode r ðkrTÞ ¼ q ð8Þ

@t

material.

resp.

The last part is represented by small frequencies below 100 Hz.

At these low frequencies, the impedance is formed by the @rC p T

capacitance, in this case the non-ideal, represented in the r ðkrTÞ ¼ s þ jrFþ j2 þ s jrF j2 þ q_ ECh þ q_ short ð9Þ

@t

Fig. 6. Schematic representation of Li-ion mass transfer phenomena which occur in Liion battery electrodes and their respective Nyquist plots. [13].

26 P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31

and

r ðs þ r’þ Þ ¼ j ð10Þ dðsocÞ IðtÞ

¼ ð17Þ

dt 3600Q Ah

resp.

For a given battery, the open circuit voltage, resistors

r ðs þ r’þ Þ ¼ ðjECh jshort Þ ð11Þ

resistances, and capacitors capacitances are functions of the

and battery state of charge (SOC) (it was measured by 0, 25, 50, 75 and

100 % SOC). These functions could be expressed in The ﬁfth order

r ðs þ r’þ Þ ¼ j ð12Þ Polynomial form:

resp.

Rs ¼ rs0 þ rs1 ðsocÞ þ rs2 ðsocÞ2 þrs3 ðsocÞ3 þrs4 ðsocÞ4

r ðs r’ Þ ¼ ðjECh jshort Þ ð13Þ þ rs4 ðsocÞ5 ð18Þ

Cp is speciﬁc heat capacity, T is thermodynamic temperature, k is

thermal conductivity, F+ and F is the cathode- and anode-side

electric potentials, t is time, s+ a s are conductivities of positive R1 ¼ r10 þ r11 ðsocÞ þ r12 ðsocÞ2 þr13 ðsocÞ3 þr14 ðsocÞ4

and negative electrode, s þ a s are potentials of positive and þ r14 ðsocÞ5 ð19Þ

negative electrode, jECh a q_ ECh volumetric current and heat

generated by electrochemical reactions, respective jshort a q_ short

volumetric current and heat generated by internal short circuit (in R2 ¼ r20 þ r21 ðsocÞ þ r22 ðsocÞ2 þr23 ðsocÞ3 þr24 ðsocÞ4

normal conditions are these variable zero values). þ r24 ðsocÞ5 ð20Þ

Electrochemical sub-models relate the local current density to

the potential. The cell model couples sub-models to thermal and

electrical ﬁelds within the cell, integrates over multiple electrode- C1 ¼ c10 þ c11 ðsocÞ þ c12 ðsocÞ2 þc13 ðsocÞ3 þc14 ðsocÞ4

pairs [16]. þ c14 ðsocÞ5 ð21Þ

The internal model is calculated by means of the Newman,

Tiedemann, Gu, and Kim model, which is simple semi-empirical

electrochemical model. It was proposed by Kwon [17] and has been

used by [14] and [15]. C2 ¼ c20 þ c21 ðsocÞ þ c22 ðsocÞ2 þc23 ðsocÞ3 þc24 ðsocÞ4

According to these equations are the potential, temperature and þ c24 ðsocÞ5 ð22Þ

current ﬁelds calculated by means ﬁnite volume method (FVM).

In the Equivalent Circuit Model (ECM), battery electric

behaviour is represented by an electrical circuit. The numerical Voc ¼ voc0 þ voc1 ðsocÞ þ voc2 ðsocÞ2 þvoc3 ðsocÞ3 þvoc4 ðsocÞ4

model was prepared using ANSYS FLUENT system. It has adopted þ voc4 ðsocÞ5 ð23Þ

the six parameter ECM model following the work of Chen [5]. In

this model, the circuit consists of three resistors and two capacitors The energy source term comes from the contribution of Joule

(see Fig. 8). The voltage-current relation can be obtained by solving heating, electrochemical reaction heating, and the entropic

the electric circuit equations: heating:

jechem ¼ ð24Þ

Volume

and

dV1 1 1

¼ V1 IðtÞ ð15Þ I dVOCV

dt R1 ðsocÞC1 ðsocÞ C1 ðsocÞ qechem ¼ VOCV ð’þ ’ Þ T ð25Þ

Volume dT

dV2 1 1 VOCV is the open circuit voltage.

¼ V2 IðtÞ ð16Þ

dt R2 ðsocÞC2 ðsocÞ C2 ðsocÞ The global parameters of thermal conductivity, speciﬁc heat

capacity, electrical conductivity, density and length parameters of

the battery were determined [18]. For calculation of effective

values of material density, thermal conductivity and speciﬁc heat

capacity, the following equations are used:

p p n n

0; 5xpc dc þ xpe de þ xs ds þ xne de þ xnc dc

xeff ¼ ð26Þ

dtotal

and

material (density, speciﬁc heat capacity, thermal conductivity) and

it is function of the material thickness. Indexes c, e and s denote

current collector, electrode and separator and indexes p and n

denote positive or negative electrode. dtot is the total thickness of

Fig. 8. Equivalent circuit model (ECM) which is used for numerical modelling the the specimen (see Fig. 9 and Table 1).

lithium ion battery [16].

P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31 27

Fig. 9. The process of simplifying the layers of a real battery into a homogeneous MSMD model [20].

Table 1

Dimensions and properties of the measured battery.

Zone Pc Pe S Ne Nc Total

d [m] 8.40E-04 2.44E-03 9.24E-04 4.28E-04 1.05E-04 8.52E-03

Density [kg m3] 2700 1500 492 2660 8900 8.04E+02

Speciﬁc Heat capacity [J (kg1 K1] 903 1260 1978 1437 385 6.94E+02

Thermal conductivity [W (m1 K1)] 238 1.48 0,334 1,04 398 1.47E+01

Electrical conductivity [S m1] 3.89E+07 1.00E-06 1.00E+04 6.33E+07 r_p 1.92E+06

r_n 3.90E+05

p p

0; 5s pc dc þ s pe de

sp ¼ ð28Þ

dtotal

and

n n

0; 5s nc dc þ s ne de

sn ¼ ð29Þ

dtotal

The simulation model accepts the Multiscale physics from sub-

micro scale to battery dimension scales [19].

Table 1 contains the measured values of the thicknesses of the Fig. 10. Dismantled KOKAM battery.

individual battery layers after disassembling and the values of

density, speciﬁc heat capacity, thermal conductivity and electrical

conductivity calculated using the equations 26–29. Materials,

which was used for calculation of battery physical properties was:

anode Aluminium, cathode Copper, separator polyethylene,

cathode material LiNi0.33Mn0.33Co0.33O2 and anode material

Carbon.

Where Pc is positive current collector, Pe is positive electrode, S

is the separator, Ne is negative electrode, Nc is negative current

collector.

curves Fig. 11. Block diagram of measuring cell.

were used for electrochemical testing and preparation of physical- CCCV was always used as a battery charging method. The

mathematical model. charging current was set to 0.2C (800 mA); cut-off voltage to 4.2 V.

The ﬁrst battery was disassembled and the dimensions of its The potentiostat was switched to the CV mode upon reaching 4.2 V

parts have been measured and used for the model preparation (see and charging continued until the current dropped below 200 mA.

Fig. 10). Subsequently, the tested battery was discharged by currents of

The second battery was connected to the potentiostat Biologic 0.2C (0.8 A), 0.5C (2 A), 1C (4 A), 2C (8 A) and 4C (16 A). Discharge

Science Instruments1 VMP31 with a booster (Block diagram is characteristics were always recorded during discharging.

represented in Fig. 11).

28 P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31

Fig. 12. Nyquist diagram of impedance measuring the KOKAM battery by different SOC.

Table 2 Table 3

The parameters of equivalent circuit model by discharging. The parameters of equivalent circuit model by charging.

SOC [%] Voc [V] Rs [V] R1 [V] C1 [F] R2 [V] C2 [F] SOC [%] Voc [V] Rs [V] R1 [V] C1 [F] R2 [V] C2 [F]

1 4.195754 0.01889 0.001540 1.241 0.002314 4.626 1 4.19785 0.01879 0.002278 4.6990 0.001542 1.266

0.75 3.920000 0.01889 0.002425 4.378 0.001645 1.193 0.75 3.94147 0.01878 0.002328 3.9170 0.001466 1.259

0.5 3.790000 0.01889 0.003286 4.734 0.001850 1.181 0.5 3.80990 0.01885 0.003221 4.4160 0.001751 1.189

0.25 3.678890 0.01895 0.002222 1.281 0.007209 5.312 0.25 3.72448 0.01889 0.002096 1.2520 0.006020 5.118

0 3.008480 0.01902 0.002970 1.591 0.021300 4.857 0 3.02384 0.01906 0.003355 1.5710 0.022690 4.880

Fig. 13. The polynomial functions obtained by discharging (dotted line ﬁtted, full line measured).

P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31 29

Fig. 14. The polynomial functions obtained by charging (dotted line ﬁtted, full line measured).

5. Parameters extraction were then inserted into the graphs and interleaved by the 5th order

polynomial function. In this way, we have obtained equations

The values of the equivalent circuit parameters were extracted describing the behaviour of the battery in different charging/

from EIS measurements using the ﬁtting program that is included discharging state (Fig. 13).

in the Biologic booster. The ﬁtted circuit was chosen according to The battery circuit parameters obtained in this way were

the mentioned equivalent circuit in Fig. 8. For the results of these inserted into the numerical model. The charging and discharge

measurements, it is important in which state of charge the battery curves of the battery were modelled and compared with the curves

is at the beginning of the measurement. measured at the laboratory measurement.

The Nyquist diagram (see Fig. 12) shows the impedance

measurement at different battery SOC using the EIS method in 6. Results and discussion

laboratories.

The obtained curves were then ﬁtted to an equivalent circuit The actual comparison of the discharge characteristics is shown

identical to the circuit shown in Fig. 8 above. Thanks to this in Fig. 14. It is obvious that the curves have the same course and are

imitation, the parameters R and C (Tables 2 and 3) were obtained slightly offset. This 0.1 V spacing is not essential to affect too much

and then were used in Eqs. (18)–(23) above. These dependencies the properties of the simulated battery and can be considered

Fig. 15. Comparison of measured and simulated discharge curves of the battery.

30 P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31

Fig. 16. Comparison of measured and simulated charge curve 0.2C of the battery.

satisfactory, particularly for copying the same waveform as the this method it can be stated that, within the tolerance of a certain

measured battery. It is necessary to realize that the battery degree of inaccuracy, it has proved to be an effective tool for

represents an ideal RC circuit. Some parameters represented by the obtaining a battery model at the RC circuit level. The use is

Nernst and Butler-Volmer equations are neglected. unambiguously where we do not know the exact properties of the

Discharging by 4C can be deﬁnitely considered as fast materials in which the batteries are composed. Conventional

discharging for example: Maximum NCR18650B discharge limit methods of battery microstructure modelling are based on often

is 2C under continuous current load or KOKAM SLPB7570180 10.6 complex electrochemical models. These models are loaded with

Ah with maximal continuous discharge 3C. errors already at the time of determining some of the coefﬁcients

The charging characteristics were measured as well as the of the given materials.

accuracy of the previous measurements. To simulate battery When modelling a particular device (electric vehicle, electric

charging, input data was used as described above. The charging train, etc.) when looking at a battery in a microstructure is not

current was set to 0.2C, which ensures a slow but still kindly charge important, replacing the battery with the model thus obtained is

of the battery (see Fig. 15). sufﬁcient. In principle, we are able to obtain a solution for any

Numerical model allows us to display some physical ﬁelds. discharge current by approximation. However, as soon as we

Fig. 16 shown the potential distribution at the positive and exceed a certain amount of discharging current, the endothermic

negative electrode at the end of discharging (Fig. 17). reaction battery begins to run. This model is unable to capture it.

But the temperature ﬁeld can be captured. Therefore, it is also

7. Conclusion important to monitor this parameter and not exceed the

manufacturers declared permissible values.

The method presented in this paper, which is suitable for the The presented process of numerical modelling was compared

extraction of lithium ion battery parameters, is called electro- with real-time measurements, which yielded satisfactory model

chemical impedance spectroscopy. In assessing the suitability of match and exact results.

Fig. 17. Potential distribution at the positive (left) and negative (right) electrode.

P. Vyroubal, T. Kazda / Journal of Energy Storage 15 (2018) 23–31 31

Acknowledgments [7] A.A. Andreev, et al., Simulation of lithium battery operation under severe

temperature conditions, Procedia Eng. 129 (2015) 201–206.

[8] D. Linden, T.B. Reddy, Handbook of Batteries, McGraw-Hill, Michigan, 2002.

This research work has been carried out in the Centre for [9] N. Nitta, F. Wu, J.T. Lee, G. Yushin, Mater. Today 18 (2015) 252.

Research and Utilization of Renewable Energy (CVVOZE). Authors [10] B. Scrosati, J. Solid State Electrochem 15 (2011) 1623.

gratefully acknowledge ﬁnancial support from the Ministry of [11] M.S. Whittingham, Chem. Rev. 104 (2004) 4271.

[12] R.J. Brodd, M. Doeff, in Batteries for Sustainability, Springer, New York, p. 5.

Education, Youth and Sports of the Czech Republic under NPU I [13] N. Williard, W. He, C. Hendricks, M. Pecht, Energies 6 (2013) 4682.

programme (project No. LO1210) [14] Y. Fernández Pulido, C. Blanco, D. Anseán, V.M. García, F. Ferrero, M. Valledor,

Measurement 106 (2017) 1–11.

[15] M. Itagaki, K. Honda, Y. Hoshi, I. Shitanda, F. Ferrero, M. Valledor, J. Electroanal.

References Chem. 737 (2015) 78–84.

[16] Tiedemann, S. Newman, Gross Editor. “Battery Design and Optimization.”

[1] P. Vyroubal, J. Maxa, T. Kazda, J. Vondrak, ECS Trans. 48 (2014) 289. Proceedings, Electrochem. Soc. Princeton, NJ, 79-1, 39, (1979).

[2] P. Vyroubal, T. Kazda, et al., Int. J. Electrochem. Sci. 11 (2016) 1938–1950. [17] K.H. Kwon, et al., J. Power Sources 163 (2006) 151.

[3] P. Vyroubal, Tomáš Kazda, R. Bayer, FEM Model of the Lithium Ion Battery Nail [18] U.S. Kim, et al., J. Electrochem. Soc. 158 (2011) A611.

Test ECS Trans. 74 (1) (2016) 71–75. [19] U.S. Kim, et al., J. Power Sources 180 (2008) 909.

[4] L. Cai, R.E. White, J. Power Sources 196 (14) (2011) 5985–5989. [20] H. Gu, Mathematical Analysis of a Zn/NiOOH Cell, J. Electrochemical Soc.

[5] M. Chen, G.A. Rincon-Mora, Accurate electrical battery model capable of Princeton, NJ. 1459-1, 464, (1983).

predicting runtime and I-V performance, IEEE Trans. 21 (2) (2006) A154–A161.

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