ISSN 1023-1935, Russian Journal of Electrochemistry, 2006, Vol. 42, No. 5, pp. 506511.

MAIK Nauka /Interperiodica (Russia), 2006.

Published in Russian in Elektrokhimiya, 2006, Vol. 42, No. 5, pp. 567573.

Approaches to the Study of Electrochemical Process Instability:

A Review*
T. Z. Fahidyz
Department of Chemical Engineering, University of Waterloo, Waterloo, ON N2L 3G1 Canada
Received May 11, 2005

AbstractThis paper summarizes experimental and theoretical investigations conducted by the authors
research group, prior to his official retirement, on various aspects of electrochemically induced convective-flow
and oscillatory instability and the stability of electrochemical reactors.
DOI: 10.1134/S1023193506050089
Key words: electrochemical instability, convective instability, oscillatory instability, instability in electrochemical reactors

INTRODUCTION
Instability is a word of many meanings. It can be
interpreted as permanent motion never reaching a final
steady state, or irregular trajectories generated by propagation patterns, etc., and, in general, any state of
inconstancy. In this paper, instability is confined to
oscillatory behavior and waves, liquid flow, and electrochemical reactor dynamics due to internal or external generating factors. The objective is to provide an
overview of intensive experimental and theoretical
projects carried out during the fourth quarter of 20th
century by the authors research group. During these
years, important new horizons of modern electrochemistry were opened up in this domain also by research
teams operating elsewhere.
The group conducted its investigation of instability
phenomena via a two-prong program. Firstly, flow
visualization techniques based on dyes and laser illumination were developed to study electrode reactioninduced spatiotemporal convective flow propagation in
liquid media. The study of the effect of externally
imposed magnetic fields on such patterns has specifically enhanced current understanding of magnetohydrodynamic (MHD) interactions with electrolytic processes with particular respect to the operation of magnetoelectrolytic reactors. In the second avenue of
research, pathways of theoretical analysis were opened
by an extensive pursuit of the application of (classical)
Lyapunov stability theory, and more recent techniques
of nonlinear dynamics, e.g., phase-plane methods, fractional Brownian motion (FBM) theory, and bifurcation
theory. A major, and by no means unexpected, result
that electrochemical instability phenomena are not
* The text was submitted by the author in English.
z Authors email: t.fahidy@engmail.uwaterloo.ca.

fully explained by purely theoretical models, attests to

the challenging complexities of the subject matter, and
the need for continuing research into it [1].
EXPERIMENTAL INVESTIGATIONS
Oscillations and fluctuations with amplitudes confined in space do not represent instability in a strict
mathematical sense, but they usually indicate nonadventitious physical influences on an otherwise stable
process. Oscillatory response to regular periodic excitation may signify instability, e.g., in the case of magnetoelectrolysis with rough cathode surfaces under
imposed periodic magnetic fields [2].
Convective flow instability generated at an electrode
surface by changing the interfacial pH due to passage of
current was extensively examined by means of
chemoanalytical indicators tagging the convecting
elements due to their characteristically dark color at
alkaline pH values [3]. A subsequent series of investigations [35], including several cathode geometries [6]
and inclined cylindrical electrodes [7], confirmed the
enhancing effect of coupled electric and magnetic fields
on vortex formation and convective flow propagation.
Computer-based image processing techniques combined with layer illumination via low power (about 250
mW) laser sheets provided an excellent tool for the
monitoring of vortex and solid-particle propagation
accompanying anodic dissolution and precipitate formation [8].
Oscillatory anodic currents, observed during the
dissolution of copper into cyanide ion-carrying electrolytes, exhibit characteristic patterns and are highly sensitive to magnetic field imposition [9]. Time series, e.g.,
FBM methods [10] employing Pox diagrams [11] were
employed in the evaluation of numerous experimen-

506

APPROACHES TO THE STUDY OF ELECTROCHEMICAL PROCESS

tally observed oscillation patterns [1218] accounting

also for the nature of the electrolyte [19]. Significant
impetus to oscillation analysis was gained by the adaptation of confocal image processing [20] and laser bombardment [21, 22] of electrodes. The spilling of electrolyte over a partitioning wall is perhaps the most dramatic manifestation of instability generated by surface
waves in a coaxial cylindrical magnetoelectrolytic cell
[23].
THEORETICAL INVESTIGATIONS AND
MODELS
Convective flow and parametric instability. On
account of its intrinsic complexity, MHD-induced convective flows can be traced mathematically only to a
limited extent by means of fundamental physical laws
[24, 25]. Arguments based on the nonzero nature of the
rot(j B)/ term (, fluid density) in the vorticity equation [26, 27] applied to the electrode/electrolyte interface layer predict qualitatively the existence of unusual
propagation patterns. The cross product of the current
density vector j and the magnetic flux density vector B,
called the MHD body force density, and a fundamental
quantity in MHD theory, is nonzero due to the nonuniform spatial distribution of its component vectors in the
interface layer. Their progressively increasing nonuniformity during the passage of electric charges is
responsible for the snowballing nature of vortex formation and propagation.
Oscillatory instability. The nature of FBM-based
analysis was briefly explained in [17, Section 3.6] and
in Appendices A and B of [15]. The Hurst exponent H
[11], determined from the slope of a logarithmic plot of
rescaled range R/S of time series data versus time lag s
is a quantitative measure of long-term correlation in a
fluctuating time series. It is also a fundamental parameter in the kernel of the definition integral of a random
function BH(t) of time [28]:
t

BH

1
= B H ( 0 ) + --------------------------- ( H + 1/2 )

K ( t u ) dB ( u )

K (t u) = (t u)

H 1/2

H 1/2

0ut
H 1/2

y7
y1

y5

yT
y6

y4

y2

y3

A
T

t1

t2

t3

t4

t5

t6

t7

Fig. 1. Qualitative illustration of the first phase of constructing a Pox diagram. Ordinate positions y1, y2, etc. are read at
-equidistant times t1, t2, etc., past arbitrary time instants T.
The lag is s = 7.

showing a window between positions A and B. The

window represents either a single period of a recurring
pattern or the entire observation span. The delay parameter s is varied in order to establish a set of uniformly
spaced time instants ranging to the lag s: t1, t2, for
every arbitrarily chosen time instant T (in Fig. 1, s = 7;
hence, t1= T + , t2 = T + 2, etc.). The rescaled range
is the ratio of
R = maxi cT(i) minicT(i)

(3)

to

where is the gamma function, and

K (t u) = (t u)

(1)

507

u<0

(2)

Within the 1/2 < H 1 domain of persistence, temporal observations are positively correlated, whereas
0 < H < 1/2 denotes the domain of antipersistence; H =
1/2 corresponds to a purely random (Gaussian) process,
and as H approaches zero, the chaotic tendency of an
oscillation or fluctuation becomes increasingly stronger.
The calculation of H is based on the construction of
the Pox diagram from experimentally observed fluctuations. The latter is illustrated qualitatively in Fig. 1
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Vol. 42

2 1/2

x i x i

i
i
S = --------------------------------------2
s
s

(4)

where the associated ranges

i

cT ( i ) =

(x

x T ); i = 1,s

(5)

j=1

portray deviations of the observation increments xi =

yi + 1 yi from the mean of observations, and s2 is the
variance of observations. The slope of a typical Pox
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FAHIDY

[37, 38]. The gist of the method is illustrated in the

Appendix using a relatively simple example of a
lumped-parameter autonomous two-dimensional system.
In an electrochemical reactor with a single-electrode
process, the two state variables may be taken as active
ion concentration and electrolyte temperature (a rational and convenient, but not an obligatory choice). Since
the reactor is driven by current, it is nonautonomous,
and its Lyapunov functions require a more involved
form with respect to the Appendix. Stability conditions
for the continuous-flow stirred tank electrolytic reactor
(CSTER) model were studied [3941] via the
Lyapunov function

log(R/S)
1.0

0.8

0.6

Slope: H 0.78

0.4

V ( x, t ) = x Qx + M ( ) d
T

0.2

(6)

0.6

0.8

1.0

1.2

1.4
log(s)

Fig. 2. Quantitative illustration of the second phase of constructing a Pox diagram. Oscillogram readings for various
time instants T are collected for specified lag values and
plotted on a logarithmic scale in term of the rescaled range
R/S (equations (3), (4)). Least-squares properties of the
regression line: coefficient of determination, 0.94; RMS of
deviations, 0.0094; slope, 0.7774; intersection, 0.25486.

diagram, illustrated in Fig. 2, yields H 0.78, indicating mediumstrong persistence.

Experimental data [9, 1222] provide considerable
evidence for H being confined to the domain of persistence in the investigated systems. The cyclic formationdissolution process involving CuO, Cu2O, CuCl or
CuBr, and CuSCN species is responsible for oscillations, but their exact role in determining the magnitude
of the Hurst exponent is not known. Analyses based on
the phase portrait/Poincar map approach [18, 2931],
low-order Fourier expansions [18, 32], and BoxJenkins differencing of time series [13, 33] suffer from the
same limitations.
A study of morphological instability of a planar
metal electrode under potentiostatic electrodeposition
and electrodissolution [34] underlines the predominant
role of kinetic effects throughout the entire potential
range, including the limiting plateau. Mapping of
parameter regions with a specific number of solutions
[35] and different types of bifurcation diagrams demonstrate the usefulness of singularity theory for the analysis of complex electrodeposition of metals, e.g., zinc
[36].
Instability in electrochemical reactors. The subject
matter was intensively studied in the early 1980s by
means of the celebrated stability theorems of Lyapunov

with positive definite matrices Q and M. This and a

more incisive analysis [42] including electrolytic alloy
deposition [43] and codeposition of two metal species
[44] underline the necessity of knowing the dependence
of electrolyte parameters and heat transport characteristics on temperature and concentration for a full utilization of Lyapunov analysis.
Considerably more challenging is the stability analysis of plug flow electrolytic reactors (PFER) and electrochemical reactors with axial dispersion (ERAD).
The challenge arises from their distributed parameter
nature requiring spatiotemporal governing equations
for the concentration and temperature profile along the
dominant space coordinate [4547]. Following the
path-finding work of Zhubov [48], Berger and Lapidus
[49], and Weigand [50], Lyapunov functionals of the
form
1

V =

w S ( )w d;
T

z/L ,

(7)

were employed to explore the size of AS regions, and

regions of indeterminate stability, in terms of the state
variable vector w and positive-definite symmetric
matrix S. They are functions of the dimensionless axial
coordinate z/L, where z is the axial coordinate and L is
the active length of the reactor [51, 52].
Figure 3 demonstrates the involved nature of stability conditions in the case of an electrochemical reactor
obeying the ERAD model. A (sudden) perturbation in
electrolyte concentration and/or temperature in regions
marked S with respect to its steady state will eventually
lead the reactor back to its steady-state position. If the
perturbation point is located, however, in regions
marked I, the Lyapunov function in equation (7) is incapable of predicting stability or lack of it. Stability
behavior is expectably affected by the direction of perturbation in temperature: the corresponding stability
condition expressed by equation (30) in [52] incorpo-

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APPROACHES TO THE STUDY OF ELECTROCHEMICAL PROCESS

rates the exothermic or endothermic nature of the electrode reaction.

Electrochemical reactor instability due to resonance. The PFER can also be described in terms of
transfer function models written for any arbitrary axial
position [53]. The practically more interesting Gc(s, L)
transfer function, related to the PFER exit, predicts an
oscillatory frequency response of both gain amplitude
and phase angle. The gain-magnitude resonant frequencies are given by the implicit relationship
sin ( )
2
------------------------------------------- = ----------------2
2
cos h ( ) cos ( )
+

CONCLUSIONS
The success achieved in the two major avenues of
instability studies, discussed in the preceding, bears
witness to the dedication and competence of numerous
graduate students and researchers of post-PhD status,
with whom the author had the privilege to collaborate
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Vol. 42

T > TS

I
S

(8)

where = Tdf is the angular frequency related to physical frequency f, and is a parameter carrying physical
characteristics of the reactor and its transportation lag
Td (the ratio of reactor length to the linear velocity of
the electrolyte). Equation (8) applies to the specific
case of a constant current across the reactor axis at
steady-state conditions. In a practical PFER, is
expected to be very small; hence, cos h ( ) 1, and
equation (8) predicts the first three resonance positions
at excitation frequencies 1.71/Td, 9/Td, 15.45/Td,
approximately. The distance between increasing resonance frequencies becomes progressively smaller.
Resonance-related local instability was shown to be
approximately predictable by the Guillemin frequency
transfer function approach [54] on the basis of experimental system step responses subjected to a number of
differentiation steps to obtain an aperiodic modulated
impulse train. Various ramifications of the technique
[5557] make it, at least in principle, attractive for the
study of reactors which do not fit physically any particular a priori mathematical model.
Electrochemical reactors subjected to random perturbations. The instability problem may be defined as
the widening of the variance of a performance measure
(e.g., active ion concentration and electrolyte temperature) in the exit stream from a reactor, with respect to
the variance of a random input (e.g., inlet active ion
concentration and current) [58]. Using the system
dynamics framework [59, 60] provided by fundamental
principles [6165] of random function theory, electrolyzer behavior was analyzed in terms of autocovariance
functions for batch, CSTER, and two-element CSTER
cascade in the case of white noise, Markovian, and
quasi-Markovian fluctuations [66]. The approach indicates that tank electrolyzers are asymptotically widesense stationary when subjected to bounded stationary
random perturbations.

509

P
C

T < TS

I
TS

Fig. 3. Phase-plane portrait for the ERAD model. C, dimensionless concentration; , electrolyte conductivity; T,
dimensionless electrolyte temperature; Ts, dimensionless
steady-state temperature; P, critical point.

over many years. Their fresh ideas and experimental

skills were highly instrumental in contributing, even if
in a modest manner, to modern electrochemical science
and engineering.
ACKNOWLEDGMENTS
Authors work was supported by the Natural Sciences and Engineering Research Council of Canada
(NSERC) and the University of Waterloo. The author is
grateful to Prof. A.D. Davydov of the Frumkin Institute
of Electrochemistry, Russian Academy of Sciences, for
his kind invitation to submit this paper.
APPENDIX
The dynamic equations for an autonomous twodimensional (2D) system
d x1
-------- = f 1 ( x 1 , x 2 ),
dt
d x2
-------- = f 2 ( x 1 , x 2 )
dt

(A.1)

possess critical points defined by the condition f1 = f2 = 0

in 2D state space (phase plane), in terms of state vector
x with its elements x1 and x2 being the state variables. If,
at a critical point x0, a positive-definite function V(x)
satisfies the conditions (i) V(x0) = 0; (2) V(x) > 0, x
x0,
at all times; and (iii) dV/dt = xgrad(V) < 0, x
x0, x R,
then the system is asymptotically stable (AS) within
space R, with reference to the critical point x0. If R is the
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FAHIDY

entire vector space (i.e., lim V(x)

, as x
),
the system is asymptotically stable in the large ASL.
2

For instance, the Lyapunov function V = x 1 + x 2

predicts that the system dx1/dt = x2, dx2/dt = x1 2x2
with single critical point (0, 0) is ASL, inasmuch as V is
positive in the entire space, it grows to infinity as either
2
x1 or x2 reach infinity, and dV/dt = = 4 x 2 is negative
everywhere. This result is borne out also by the
repeated negative eigenvalues of 1, or equivalently,
due to the negative trace and positive determinant of the
system matrix A with elements a11 = 0, a12 = 1, a21 = 1,
a22 = 2.
Indeterminacy arises when the dV/dt < 0 condition
(or its violation) cannot be established. For instance,
3
4
the stability of the system dx1/dt = x 1 x2, dx2/dt = x 1
with critical point (0, 0) is impossible to ascertain with
2
2
V = x 1 + x 2 , because dV/dt = 0 in the entire state space.
2n

However, the generalized function family V = x 1 +

2n

x 2 , n = 1, 2, 3, , would predict widely different

regions of asymptotic stability. In this situation, the
dV/dt < 0 condition is satisfied by the inequality
2(n 1)
2(n 1)
x2 [ x 1
x2
] > 0.
Among an infinite, in principle, number of possible
Lyapunov function candidates, the quadratic forms V =
xTPx and V = f(x)TIf(x) (the latter is widely known as the
Krasovskii function [67]) were particularly successful;
P is an a priori undefined symmetric positive definite
matrix, and I is the identity matrix (the simplest positive definite symmetric matrix). The Krasovskii-type
Lyapunov function tends to predict an RAS of conservative size.
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