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Issued and by ZAHNER-elektrik GmbH & Co. KG in June 2002

… we have to say sorry for the long time you had to scientific presentations.

wait for this new issue of Electrochemical Applica-

tions. The delay was mainly caused by two facts: on The recent issue of Electrochemical Applications does focus

the one hand we developed a lot of new products like not only on EIS but on associated methods which are

the high current potentiostats of the EL- and the PP- able to complement EIS in specific applications. First

series, the NOISE probe with outstanding features of all, there is the HCI (High Current Interrupt)

(not only for noise measurements) and the new PC method, which allows you to find results in low im-

interface which is running under Windows95/98 as pedance objects such as power generating devices

well as under WindowsNT/2000 now. On the other even at high frequencies. The relaxation voltammetry

hand we had a lot of scientific presentations at well- is an alternative method for investigating high imped-

known meetings which yield enough stuff for the next ance systems such as coatings. The EIS chapter of

issues of Electrochemical Applications. this issue comes from Dr. Hoffmann (MTU-

Friedrichshafen GmbH) who is demonstrating the

Due to these facts we increased the Zahner team, application of AC impedance spectroscopy on molten

and I am proud to introduce to you Dr. Werner carbonate fuel cells.

Strunz, our new co-worker. He studied chemistry in

Heidelberg, Germany and took his doctor’s degree on We hope, the topics of this issue are a good excuse

“Electrical Conducting Coordination Polymers“. He is for the long waiting period.

supporting the Zahner team in several software pro- Your Zahner Team

jects and – above all – he is enhancing our scientific

Measuring low impedances at high

performance of the device and accounts some-

frequencies times for the main part of the overall losses. It

is very sensitive to degradation caused by corro-

F. Richter, Siemens AG, KWU, Erlangen, Germany, sion and thermal stress.

franz.richter@erl11.siemens.de

an o de

C.-A. Schiller, Zahner-elektrik, Kronach, Germany, c o n n e c to r

in d u c ta n c e

cas@zahner.de an o de

re s is ta n c e

norbert.wagner@dlr.de an o de

F a r a d a y ic a no de a n o d e s id e

proc es s * d o u b l e la y e r * po rou s

in s id e t h e c a p a c ita n c e d i s tr ib u te d

If a power generating device is examined, its dynamic p o ro u s

s y s te m

im p e d a n c e

work which represents anode, cathode, membrane, m e m b ra n e +

e le c t ro ly te e q u iv a le n c e total

o h m ic

re s is ta n c e los s

electrolyte, and connectors.

b u lk total

in d u c ta n c e i n d u c tiv e

s h are

The specific losses of every partial impedance of the

c a th o d e

network contribute to the overall efficiency of the F a r a d a y ic

proc es s c a th o d e

c a th o d e s id e

po rou s

device. The porous layers of anode and cathode, in s id e t h e

p o ro u s

* d o u b l e la y e r

c a p a c ita n c e

* d i s tr ib u te d

im p e d a n c e

c o n n e c to r

much less important. There is the resistance of the re s is ta n c e

c o n n e c to r

of contacts and connectors. A dynamic part is added in d u c ta n c e

Fig. 1: Simplified electrical equivalent circuit of a

Nevertheless, the ohmic part (electrolyte, membrane, typical electrochemical power source device

connectors) plays an important role regarding the

Represented by TEST SOLUTIONS (770)410-9166 http://www.test-solutions.biz

Electrochemical Applications 1/02 page 2

In applications with dynamic load changes the induc- It is rather contaminated by dynamically induced

tive parts, for example in a laptop computer battery or error voltages. These errors are caused by unavoid-

in electromotive applications, are limiting the maxi- able mutual induction from the magnetic field of the

mum pulse load available. current circuit.

and with the strength of the magnetic field of the

- imaginary part

c a th o d e a rc

current. It depends on the geometry and grows with

the dimensions of the object. For the investigation of

a n o d e a rc power sources this means: The more you scale up,

the lower is the available upper frequency limit (fg).

Finally, there is a limit for the EIS at low ohmic ob-

jects. At a rough estimation you can calculate with:

L⋅ ω re a l p a rt

R fg ≈ 1 MHz * |Z|min / Ohm

a n o d e s id e c a th o d e s id e

p o ro u s to ta l to ta l

in d u c tiv e O h m ic

p o ro u s As a consequence, the window for getting an Ohmic

d is trib u te d d is trib u te d

im p e d a n c e s h a re lo s s im p e d a n c e resistance information by means of the EIS gets

smaller for bigger cells. For certain systems, the

L R window will be closed.

*

. these conditions? The question is answered by the

Fig. 2: The appearance of ohmic share and stray induc- well known current interrupt technique, which does

tance in a fuel cell spectrum not need the knowledge of two signals simultane-

ously. The principle is depicted in figure 4 and ex-

EIS allows to separate all contributions and to deter- plained in the following:

mine the ohmic part in the high frequency region of a

spectrum, where the impedance curve intersects the elec tro nic s w itc h po ten tia l

real axis. The inductance is shown at successive m e as ure m en t

higher frequencies in the diagram. But there is one

great restriction: Measuring impedance always

means to measure two signals, current and voltage.

∼

* E

Z = ∼

∼

I I

loa d o bjec t

∼

E

s tea dy s ta te

c u rre nt I

ze ro c urr en t

Z = I m p e d a n c e o f t h e O b je c t o f In t e r e s t

W i th th e E x te n s i o n s in S p a c e x , y , z .

C u rre n t line ar

∼ s tep ∆ E

E n o is e ∝ ω , x, y, z, I p o ten tial

u n de r loa d O hm ic s h are =

I n te r f e r in g ∆ E

Current Flow

P o te n ti a l

E n o is e 1 tim e o f I

in te rru p tio n T im e

Interesting

P otential

Z P o te n t ia l

C o u p l.

mine the ohmic share

I n te r f e r in g

P o te n ti a l

E n o is e 2

A steady-state current is interrupted by a switch. The

step response of the potential is sampled and ana-

lysed assuming that the current drops instantane-

Fig. 3: Basic impedance measurement circuit – ously from its stationary value to zero.

principle (top) and detail (bottom)

In practice, the settling time depends on the electro-

A closer look at the circuit in figure 3 shows that the magnetic energy stored in the parasitic capacity and

potential information does not only contain the inter- inductivity of the cell arrangement on the one hand

esting part from the site of the connecting terminals. and the damping process on the other hand.

Electrochemical Applications 1/02 page 3

Provided that the set-up is built appropriate, the inter- spectrum and all parasitic effects can be analysed by

ruption results in a breakdown of the current to at means of EIS methods.

least small values within a short time. In this case,

total total

the potential will be disturbed much less by mutual porous damped

total

Ohmic

induction compared with an EIS measurement. distributed

impedance

inductive

share

share

pedance can be easily seen from the height of the

*

fast rectangular step of the potential. For the evalua-

tion a linear step model is commonly used.

E /m V T im e / µ s C sw

R dmp R sw

0

-5 0 C sw,R : Capacitance

sw and resistance of the electronic switch.

R dmp: Damping of the inductive share due to spatial distribution.

-1 0 0

-1 5 0

current interrupt measurement set-up of an electrochemi-

cal power source device.

-2 0 0

In figure 6, a simplified equivalent circuit for a com-

E /m V T im e / µ s plete HCI measurement set-up of a power cell is

shown. It contains the impedance of the active cell

0

part (circle), the integral inductance (L) and resis-

tance (R) and the parasitic effects of the switch cir-

-5 0

cuit. The resonance circuit is mainly built of the series

inductance, the double layer capacity and the capac-

-1 0 0

ity of the electronic switch. It is responsible for the

overshot and “ringing” in the pulse response signal.

-1 5 0

T im e

I E

-2 0 0 E (t)

10 15 20 I0 fro m

c alib ra tio n

I(t) E0 pro c e du re

Fig. 5: Typical current interrupt potential step response. 0

cell PEM fuel cell at 80 A. H a n n in g W in d o w

f(t) = E (t) ⋅ H (t)

But this evaluation suffers from the fact that the h ig h prec is ion

c oa x ia l re s is to r

analysis of the time domain data is interfered by the Z o om -F F T

“ringing” in the signal as a result of the parasitic G ( j ω ) = F (f(t))

resonance. In addition, the early phase of the re-

sponse is characterized by a non-linear behavior due A m plitud e R efe re nc e

to the imperfect characteristics of the electronic S pe c tru m S pe c trum

switch. Furthermore, the response of both double-

layers may follow soon after the interruption when the

freq ue nc y freq ue nc y

concentrations of the involved species turn from their

steady state values to new ones without load. All

S c a la r Im p ed an c e

these effects bend and distort the expected ideal S p e ctru m

shape of the potential step. Therefore, the automatic

im pedance

ple fit to a linear step model often leads to inaccurate

results. freq ue nc y

results of comparable reliability to the EIS. The basic Fig. 7: Principle scheme of the Zahner high current inter-

idea is not to evaluate the distorted step function in rupt data processing.

the time domain. Instead, after a transformation of

the data into the frequency domain, the resulting Figure 7 illustrates the essential steps for the trans-

formation of the time domain data into the frequency

Represented by TEST SOLUTIONS (770)410-9166 http://www.test-solutions.biz

Electrochemical Applications 1/02 page 4

domain. The potential response signal E is sampled pared to the automatic minimum detection in the

by a transient recorder. scalar impedance function.

The numeric algorithms use discrete Fourier trans- Figure 10 is a sketch of the practical set-up of our

form methods to achieve an effective analysis. In high current interrupt measurement arrangement of a

order to minimize the errors caused by their applica- fuel cell. The electrochemical cell (A) is supplied by

tion on single events, a weighing function has to be means of an electronic load (B) or another type of

applied. At least, a Zoom FFT calculates the ampli- high power potentiostat to force the steady state load

tude spectrum in the frequency domain. A similar conditions. Additionally, the potentiostat acts as fast

procedure using a reference resistor was done for electronic switch for the current interruption.

calibration. The quotient of both spectra finally leads |impedance| / Ω

to the modulus of the impedance of the unknown 10m

object.

|impedance| / Ω

10m 1m

f0 f1

100u

1m 1K 10K 100K 1M 8M

frequency / Hz

Zmin ⇓

η

2 π dϕ

π η∫

100u ln | Z (η) | ≈ const. + ϕ (ω )d ln ω − ⋅ (η)

6 d ln ω

1K 10K 100K 1M 8M 0

frequency / Hz ⇓

Fig. 8: Automatic evaluation of the ohmic share from the phase ο

scalar impedance function. 90

evaluate the ohmic share in a simple, automated 45

way: The user selects a reliable frequency range for

analysis, which excludes the parasitic resonance at

0

the high frequency end. The impedance minimum

within this range represents the ohmic share with an

acceptable accuracy of about 1 to 3%. -45

the standard methods of the EIS, beside the imped- -90

ance, the phase data will be necessary: For this cal- 1K 10K 100K 1M 8M

culation a relation between impedance and phase for frequency / Hz

all two pole impedance objects of minimum phase

1

can be used. The ZHIT relation allows to calculate

the modulus of the impedance course from the Fig. 9: Calculation of the phase angle from the impedance

1

course of the phase angle. It will also be able to per- modulus by means of the inverse application of the ZHIT

form the inverse application, if one uses the ZHIT in transform. The ZHIT equation shows that the impedance

modulus at the frequency η can be calculated from the

an iterative numeric way. This is the way, our analy-

integral of the phase angle course ϕ(ω) within limited

sis software obtains a complete spectrum. frequency boundaries (η 0 to η). A correction term propor-

tional to dϕ/dlnω enhances the accuracy.

The complex spectrum can now be analyzed in the

usual way, for instance, by means of simulation and

fitting of the equivalent circuit. According to our ex- The potentiostat is controlled by an electrochemical

perience, the ohmic share can be determined in this workstation (D) including a high resolution transient

way, with typically the double or triple accuracy com- recorder. The recorder input is connected to the po-

tential sense lines of the cell along a so called pulse

1

W. Ehm, R. Kaus, C.-A. Schiller, W. Strunz: ZHIT - a simple probe (C). The main task of the pulse probe is the

relation between impedance modulus and phase angle... Electro- galvanic isolation of the potential sense circuit from

chemical Society Proceedings 2000-24, 1

Represented by TEST SOLUTIONS (770)410-9166 http://www.test-solutions.biz

Electrochemical Applications 1/02 page 5

the instrument in order to minimize electromagnetic We also found that the HCI worked fine with power

interference. On the other hand, it is responsible for generating devices. As an example, the results of an

the protection of the instrument input by means of an EIS and a HCI experiment at a high temperature fuel

energy consuming clipping circuit. cell are depicted in figure 12. The cell has been

driven with air and humidified hydrogen and gener-

After a short ‘sampling shot’ during the interrupt, the ated more than four Amperes at a potential exceeding

instrument switches on the current again, in order to 0.73 Volts. In both experiments the best case

re-establish the steady state and to avoid potential

damage of the cell. The pulse response is analyzed

then by the software of the workstation as described wiring was used to reduce the mutual induction con-

before. tribution.

top of figure 12. At the bottom, the transformed im-

pedance (circles) as well as a comparative imped-

ance measurement (rhombi) are drawn. As one can

see, the methods complement each other for the

different frequency ranges. In this special case, the

frequency limit for the EIS experiment to get accurate

information on the ohmic share is not exceeded.

Therefore, both methods deliver the correct results.

impedance Ω

100m

10m Ω

30m

A

10m

10 1K 100K

frequency / Hz

Current load lines

Potential sense lines

Fig. 10: Practical set-up of a high current interrupt fuel cell phase ο

measurement arrangement

10m Ω

45

0

A lot of test experiments under controlled conditions

have been done. The major experience is that, com-

B -45

sensitive to mutual induction artefacts. This is illus- 10 1K 100K

trated by the example depicted in figure 11. Here, we frequency / Hz

made test measurements at resistors using two dif-

ferent, intentionally non-optimized connection geome- Fig. 11: Results of test measurements at reference resis-

tries. As you can see, the strong in-phase mutual tors incl. mutual induction (MI) components.

induction of the above example leads to an inductive

component which seems unrealistically high in the A: In phase MI leads to a high inductive response in the

case of the standard EIS. The HCI method, however, case of EIS (full dots) whereas the HCI spectrum (squares)

matches the theory.

leads to the almost exact value. B: Out-of-phase MI causes paradox capacitive (-) EIS

phase courses (squares) while the HCI phase course

With the other example, which shows a strong out-of- shows the correct phase sign for inductance (+).

phase mutual induction, one obtains almost the same

impedance functions, which has been omitted here.

Yet, the phase diagram shows paradox behaviour for

the standard EIS curve: The course indicates capaci-

tive characteristics! The phase curve of the HCI ex-

periment shows the correct sign due to its origin from

the ZHIT transform.

Electrochemical Applications 1/02 page 6

formed. The shift of the increase of the impedance for

100

the transformed HCI-data (circles) to higher frequen-

cies indicates the smaller sensitivity of the HCI

0 measurement against the mutual induction.

the EIS- and the HCI-data at the low frequency end of

-2 0 0 1.1 KHz results from a non-linear component in the

long term pulse response signal. HCI analysis has to

rely on the rule of linearity. The transient changes of

0 200 400 600 800

about -10 mV within the 0.85-milliseconds-analysis-

interval may be enough to violate this rule.

im p e d a n c e Ω

100m

Conclusion

30m 1. EIS capabilities are basically limited by mutual

induction at the high-frequency low-impedance edge.

This falsifies significantly the results for ohmic and

10m

inductive share.

2. The HCI capability is limited by the magnetic en-

100m 10 1K 100K ergy stored in the load circuit.

fr e q u e n c y / H z 3. The HCI analysis can be automatically analyzed

reliably by transforming the time data into the fre-

Fig. 12: High current interrupt measurement of a single quency domain.

solid oxide fuel cell at 866°C. 4. According to our experience, HCI can extend the

EIS: 100 mHz – 100 kHz (rhombi) available frequency range about a factor of three to

HIC: 1 kHz – 800 kHz (circles) ten in a carefully optimized experimental set-up.

5. HCI data interpretation should not be extended to

The last example demonstrates that the dominating the low frequency response. The unavoidable viola-

error from the unavoidable mutual induction falsifies tion of the EIS linearity rule after a certain interruption

the result of standard EIS measurements at very low time may lead to misinterpretations.

impedance objects. In the experiments depicted in 6. Thus, an arrangement which performs both, the

figure 13, a HCI measurement (top) as well as a standard EIS and the HCI measurement within one

comparative EIS measurement (bottom, triangles) set-up, is the best choice for the challenges of elec-

trochemical power source device testing.

E /m V T im e / µ s

-5 0

A B

-1 0 0

-1 5 0

-2 0 0

0 2 0 0 4 0 0 6 0 0 8 0 0

im p e d a n c e Ω

For N. American support contact:

3 m PHIL WOLF

C D TEST SOLUTIONS

1 m 5665 Hwy 9 N, Ste. 103-181

Alpharetta GA 30004

USA

3 0 0 u

T: 770-410-9166

1 0 0 m 1 0 1 K 1 0 0 K

fre q u e n c y / H z

F: 443-947-0745

C: 678-231-5783

phil@test-solutions.biz

Fig. 13: High current interrupt measurement of a single

PEM fuel cell at 85° C and 80 A. The resulting spectrum http://www.test-solutions.biz

(C) is compared with a standard EIS (D).

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