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Descrição dos métodos de impedância eletroquimica.

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Outline

The Autolab instrument

Cell connections and configurations

Basics of EIS

Practical EIS

Data analysis

Applications

The Instrument

Instrumentation requirements

for EIS

PGSTAT

Impedance analyzer

Software for data acquisition and

analysis

The instrument

1 MHz 10 Hz range with PGSTAT

connection to Windows software

FRA32M Module

Module for electrochemical impedance

spectroscopy

32 MHz to 10 Hz

1 MHz to 10 Hz in combination

with the PGSTAT

DC range: up to 10 V

Single sine and multi-sine

FRA32M

New impedance analyzer module

Replaces the FRA2

Works with Autolab PGSTAT series

Not available for AutolabIII

FRA32M

32M stands for 32 MHz

!! MAXIMUM Frequency with

PGSTAT: 1 MHz !!

Future developments to raise the limit

FRA32M

Direct DSG output

20 MHz

32 MHz

PGSTAT128N/FRA32M, 500 mV (top)

Sharp decrease @ 700

kHz

~80% attenuation @ 1 MHz

FRA32M

Uses on-board DSP

Crunches 1 M per channel down to

4096 points

And finally down to 1

Much faster than FRA2

No filtering

FRA2 vs FRA32M

FRA2 vs FRA32M

FRA32M: wrapping up

Very advanced module

Expected product lifetime 10+ years

All procedures are compatible!

The instrument

with 1 MHz 10 Hz range

connection to Windows software

Applied Frequency Resolution of 0.003%

AC amplitude: 0.2mV to 0.35 V (RMS)

Input range of 10 V

Max. frequency limited by PGSTAT

Possible configurations

PGSTAT128N, 302N, 100N, 302F

Multi autolab with FRA32M module

Autolab III with built-in FRA2

Instrumental limitations

Contour plot

Z accurately at any

frequency

Cell connections

Cell connections

Autolab potentiostat / Galvanostat

Cell connections

PGSTAT provides 4

connections

CE and WE (current

measurement)

RE and S (voltage

measurement)

interfacial potential is not critical

of energy storage and energy conversion devices

Impedance measured between RE and S

electrochemical measurements

The RE in close proximity of WE to control the interfacial

potential accurately

Impedance measured between RE and S

liquid/liquid interface (two non-miscible electrolytes or

two electrolytes separated by a membrane)

Impedance measured between RE and S

Electrochemical cell

WE/S

CE

RE

Electrochemical

interface

Electrochemical interface

Interface

Electrode

Potential

+

e-

+

+

+

+

+

+

IHP OHP

1- 100 m

OHP Outer Helholtz plane: closest ions free to move within the electrolyte

Equivalent circuit

Electrochemical interface model

Equivalent circuit

Uncompensated resistance, Ru

Solution between RE and WE

Concentration, cell setup, Temperature,

conductivity, type of ions, mass transport,

Equivalent circuit

Typical values:

up to 100 (aqueous solution)

KCl 0.1 mol/L 20C = 85.69

up to 10 k (organic solvent)

Between 1m to 1 Batteries

Equivalent circuit

Diffuse interfacial capacitance

Concentration, ions, electrode surface,

adsorbed species,

Equivalent circuit

Typical values:

Double layer bare metal

Fe2O3 - Ni2O5

Al2O3

Epoxy cast coating

Asphalt coating

10-50 F/cm2

2 F/cm2

0.5 F/cm2

6 pF/cm2

0.5 pF/cm2

Bernard Tribollet & Mark E. Orazem: Electrochemical Impedance Spectroscopy, Wiley-Interscience, 2008

Equivalent circuit

Polarization resistance

Electron transfer kinetics, Temperature,

electrode composition, morphology,

Equivalent circuit

( m very fast kinetics up to G slow

charge transfer)

Silver 1.59 10-8 m, Copper 1.68 10-8 m

Silicon 6.40 102 m Glass1010 to 1014 m

Teflon 1022 to 1024 m

Equivalent circuit

Related to semi infinite diffusion

T, concentration, diffusion coefficients,

viscosity, electrode area

Typical values: depends on the system

Electrochemical methods

Large number of methods available

DC: cyclic voltammetry, chrono

amperometry,

AC: electrochemical impedance

spectroscopy,

Advantage of DC methods

Ex: cyclic voltammetry

Most popular technique in

electrochemistry

Provides a complete overview of the

electrochemical interface

Immediately recognizable

Cyclic voltammetry

Platinum in HClO4 0.1 M

Immediately

recognizable

Cyclic voltammetry

Platinum in HClO4 0.1 M

Added EtOH

Anodic peaks attributed

to the oxidation of EtOH

Disadvantage of DC methods

System is driven away from equilibrium

Response is given by individual

contributions

Information about the rate determining

step can be determined

No information on the internal dynamics

of the system

Disadvantage of DC methods

Iron in sea water

No direct information about

electrochemical interface

Assuming a simple dummy cell

CV staircase method

Using Ohms law and a linear

regression:

Slope = 0.00014241

1/Slope = 7021.98

102 + 2230 + 4700 (7032 )

EIS

Using direct reading of data

shown in the Nyquist plot, R1,

R2 and R3 are immediately

known

R1 = 106

R2 = 4844.1106=4738.1

R3 = 7028.74844.1=2184.6

EIS

Using indirect reading of

data shown in the Nyquist

plot, C1, and C2 are easy to

calculate

max

1

R C

C1 = 9.95 nF using R2

C2 = 10.77 F using R3

Alternative: EIS

Electrochemical impedance

spectroscopy

Study of the variation of the impedance

of an electrochemical system with the

frequency of a small-amplitude AC

perturbation

Advantages of EIS

System remains at equilibrium

Non destructive method

Can be applied in many fields

Corrosion, biosensors, solar cells,

semiconductors, superpacitors, fuel

cells, batteries

EIS Basics

EIS Basics

Ohm's law gives a simple relation

between

dc-potential (E) and dc-current (i):

E

R

I

EIS Basics

EIS is a transfer function between

potential and current

et e sin t

Z()

it i sin t

e sin t

sin t

Z

Z0

i sin t

sin t

EIS Basics

it i sin t

et e sin t

The

current

response

leads or lags the voltage

by a phase angle

EIS Basics

When ac-signals are involved the

relation is:

Z ()=

E ()

I ()

It is common practice to express Z as

a complex function

Z() Z0e

j( )

Z0 cos jsin

Z ZRe j ZIm

Real components are located on the

abscissa

Imaginary components are located on

the ordinates

Nyquist plot

Plot of Z vs Z, using iso-metric

axes

Total impedance Real component Imaginary component

Nyquist

Bode presentation

Plot of |Z| vs log F and vs log F

Phase angle

Z() Z e

j( )

Bode presentation

3D projection

3D projection

Ohms law holds at all frequencies for a

pure resistor

Z() R

0

Ohms law holds at all frequencies for a

pure resistor

Z() R

0

charge transfer resistance

Resistor

Impedance (reactance) is frequency

dependent

1

Z()

C

Capacitor

Capacitor

1

1

ZC

j

jC

C

90 phase shift

Typical examples: double layer

capacitance, coating capacitance

Capacitor

Inductance

Inductance

ZL jL

90

Typical examples: instrumental

artifacts, adsorption phenomena

Inductance

RC, series

Impedance of element in series =

impedance of elements

E ER EC

i iR iC

1

Z ZR ZC R j

C

1

Z() R R

C

0

2

RC, series

RC, series

RC, parallel

Impedance of element in parallel =

1/R (1/impedance of elements)

1

1

E ER EC i iR iC

1

1

1

1

jC

Z ZR ZC R

R

Z

1 RjC

Z()

0

2

1

C

R

RC, parallel

Impedance vs admittance

Randles Cell

Electrochemical cell model

> ZCdl > 0

max

1

Zf Cdl

Capacitive

contribution

R

Pure resistive behavior,

no phase change.

R + Zf

Pure resistive behavior,

no phase change.

Randles Cell

Electrochemical cell model

R + Zf

> ZCdl > 0

Capacitive

contribution

0

Pure resistive behavior,

no phase change.

no phase change.

Randles Cell

Electrochemical cell model

Fmax

R + Zf

EIS conditions

3 fundamental conditions

Linearity

Stability

Causality

Linearity condition

The applied AC amplitude must be

small so that the response of the cell

can be assumed to be linear (in 1st

approx)

Important choice of the applied

amplitude

Linearity condition

(or current) perturbation is applied. The response of the cell is a small

amplitude sinusoidal current (or potential)

Linearity condition

linear and the response

depends on the system

Linearity condition

Linearity condition

Potentiostatic or galvanostatic control?

Z is independent of the mode

At what DC potential or current?

Always at OCP?

Depends on the system

Requires knowledge of the system

What should the AC amplitude be?

Linearity condition

FAQ # 1

How to choose the amplitude?

Small enough to stay linear

Big enough to measure a response

Stability condition

The overall state of the system should

not change (significantly) during the

acquisition of the data

Important choice of frequency range

and measurement conditions

Stability condition

Corrosion of the electrode, adsorption

or formation of oxides, discharge of

the device, changes in the

electrochemical interface,

Electrochemical system are unstable

Stability condition

Frequency scan

Experimental duration is dominated by the low frequency limit

Stability condition

Min. time for Z at 10 Hz: 10.000 s

Scan from 1 kHz to 1 mHz, 61

frequencies, log. distribution

2 h, 47 minutes (estimated)

Scan from 1 MHz to 1 Hz, 61

frequencies, log. Distribution

7 minutes (estimated)

Stability condition

Duration

The experiment

duration is dominated

by the low frequencies

Causality condition

The measured AC response of the

system must be directly correlated to

the applied AC stimulus

Important to shield the cell from

outside perturbations

Avoiding traps

Avoiding traps

Powerful method but not stand alone

Knowledge of the system is required

3 conditions must be respected

Instrument is not a black box

Measurement sequence

Step 1: AC signal is applied on the cell

Step 2: AC response is recorded

Step 3: signals are sent to the

impedance analyzer

Measurement sequence

Lissajous plot

Measurement sequence

FFT is computed for both signals

Impedance is calculated from

frequency domain data

Measurement sequence

Updated in the software

Hidden information

Nyquist and Bode plots do not show

all the information

The raw signals are insteresting to

consider

Lissajous plots test the linearity

Lissajous plots

Pure R

Pure C

Real cell

Lissajous plots

Measurement of impedance

V OA

Z

1M

i

OB

D A

OD

sin

33

OA

Lissajous plots

Easy to detect non-linear behaviour

200 Hz / 25 mV AC

20 Hz / 25 mV AC

The raw data can be

used to verify the data

quality in terms of

limit of detection

Kramers-Kronig test

Basic test for data validation

Equations linking real and imaginary

components of complex quantities for

systems fulfilling the conditions of

linearity, causality and stability

Kramers-Kronig test

Diagnostic tool for impedance data

Test the data for consistency

Recalculates the real/imaginary part

based on the measured imaginary/real

part

Kramers-Kronig test

significant deviation from calculated values indicated violation

of linearity, stability or causality condition

Practical EIS

Practical EIS

Different protocols

Frequency scan: other parameters

are fixed

Single frequency: other parameters

are changed

Combination of both

Frequency range?

Depends on the systems time constants

10 kHz to 100 mHz is a good start

(always high to low)

Above 10 kHz effects from cables,

reference electrode and connections

Frequency scan

properties

Frequency

distribution

Amplitude

Wave type

Direction: high to low frequency

low frequency (stability condition)

# frequencies and distribution:

10/decade and logarithmic

! Duration: dominated by the low

frequency

Alternative: multisine

Multisine: linear combination of

single sines

5

sines signal,

contain a base

frequency and 4

higher harmonics

Multisine: linear combination of

single sines

15 sines signal,

contain a base

frequency and 14

higher harmonics

1000 Hz 0.001 Hz, 61 Freq, single:

2h, 47 min

1000 Hz 0.001 Hz, 13 Freq, 5 sine:

50 min

37 min with 15 sines

Faster but less accurate!

Data analysis

Data analysis

Analysis: crucial part of the EIS

Different tools are available

Difficult and time consuming

Pitfall: extract too much information

Analysis tools

Find circle (quick fit): used to quickly

fit a semi-circle in the Nyquist

Provides a quick estimate using a

R(RQ) circuit

Analysis tools

Find circle (quick fit)

Analysis tools

Find circle (quick fit)

Analysis tools

Fitting using equivalent circuit

User-defined equivalent circuit built

with different elements

R, C, L, Q, etc

Parallel or series

Non-linear least-squares fit

Analysis tools

Circuit description based on

B.A.Boukamp:

Solid state Ionics 20 (1986) 31-44 &

Solid State Ionics 18&19 (1986)

136-140

Analysis tools

Elements

Analysis tools

Fitting tool comes with circuit editor

using split and join elements

Analysis tools

Initial conditions,

boundaries, fixed

parameters can be

edited in the dedicated

panel

Fitting progress

Iterative process

Several iterations

required in order to

reach convergence

Report

Non uniqueness of circuits

The 3 circuits give the

same results (identical

2 values)

Knowledge about the system is

required

EIS never to be considered as stand

alone!

Practical examples

RE

NaCl

CE

3 electrode setup

Z measured

between RE and WE

Coating

Steel

WE

Pure C

Nyquist

Bode

Pure R

RE

Interpretation?

CE

Ru

NaCl

Cdl

Coating

Steel

WE

Poor fit

Case 1 problem?

Element Q

Used to describe an imperfect

behaviour of a reactance

ZQ

1

Y0 j

ZC

j

C

n = 1 capacitor

n = 0 resistor

n = 0.5 uniform diffusion

0.5 < n < 1 rough electrode

0 < n < 0.5 porous electrode

Case 1 Element Q

Case 1 Element Q

Good fit

surface

Re

Electrolyte

Surface film

Csf

Cdl

Rct

Electrode

surface

RE

NaCl

CE

3 electrode setup

Z measured

between RE and WE

Coating

Steel

WE

Pure C

Two semi-circles

Nyquist

Pure R

Bode

Fitting?

Knowledge of the system is required

Not the same coating as case 1

What would happen if the coating

fails?

RE

CE

Ru

NaCl

Cdl

Coating

Steel

Pores

WE

Ru

Cdl

Coating + pores

Steel

Fit result

Knowledge of the system is required

when fitting the data

blisters

Electrolyte

Re

Surface film

Rep

Blister with electrolyte

Csf

Cdl

Zwa

Rct

Electrode

blisters

Electrolyte

Re

Csf1

Rsf1

Surface

film 1

Rsf2

Surface film 2

Csf2

Cdl

Rct

Electrode

Semi infinite diffusion

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3-

Semi infinite diffusion

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3-

Angle of 45

Indication of semiinfinite diffusion

Randles-like

behavior

Warburg diffusion element, W

|ZW| = |ZW|

45

- = /4

W depends on the concentration,

diffusion coefficient and temperature

ZW

j

RT

1

1

2 2

n F A 2 DO CO

DRCR

Semi infinite diffusion

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3-

Semi-infinite diffusion

contribution

Finite diffusion

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3Hydrodynamic conditions

Falls off towards a

finite impedance

Angle of 45

Indication of semiinfinite diffusion

through a thin layer, a coating

Finite diffusion layer

Typically used for:

O element

ZO

ZO

1

Y0 j

1

Y0 j

tanh B j

ZW

- Ion selective electrodes

- Diffusion through a coating

O element is identical to W

when tanh argument >

in the H2 Stream

Red O2

Blue Air

Air

O2

Finite diffusion layer

O element

B

D

RDE

electrode

Finite diffusion

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3-

Variation of rotation rate

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3At higher rotation rates

diffusion layer thickness,

decreases ZO decreases

Variation of rotation rate

Platinum working electrode

[Fe(CN)6]4-/[Fe(CN)6]3-

ZO

1

Y0 j

tanh B j

B600RPM B1200RPM B2400RPM

Tangent hyperbolic diffusion

Impedance of finite-length diffusion

with reflective boundary

Typical of film with electro-active

species, porous electrodes, Li Batteries

Y Y0 j th B j

Z ( )=

1

Y0 j

coth B j

Tangent hyperbolic diffusion

B = time (second) take for a reactant to

diffuse from one side of the layer to the

other.

Thickness of the thin layer

Diffusion coefficient D

B=

D

Tangent hyperbolic diffusion

T element

>45

Tangent hyperbolic diffusion

Chemical reaction in bulk solution

Model for porous electrodes

Lithium batteries

1

k j

Y Y0 k j

Model for porous electrodes

Li-Thionyl battery

elements

T, bounded Warburg,

linear finite diffusion

W, semi-infinite

linear diffusion

O, finite-length diffusion

T>450

W 450

Case 10 Inductance

High frequencies inductance

Low frequencies inductance

Z=jL

Wrong frequencies range, electrode

inductance, connecting wire

Adsorption process at electrode surface,

surface reaction or chemical modification

Adsorption process at electrode surface,

surface reaction or chemical modification

Case 11 Bisquert2

Transmission line element

electrode of thickness L

Case 11 Bisquert2

X3X

X3X

X1X

X3X

X1X

X1X

X3X

X1X

X2

X2

XX

X2

Case 11 Bisquert2

ZB2

X1X 2

2

12 22

L

cot anh

1 2

1 2

sinh

Where is given by

X3

1 2

Case 11 Bisquert2

DSSC V@MaxPP

Case 11 Bisquert2

DSSC V@ OCP

Resistance

Capacitance

Inductance

Y0 and n

Warburg diffusion

Y0

Finite diffusion

Y0 and B

Bound diffusion

Y0 and B

Gerischer impedance

Y0 and Ka

Transmission line

B2

R1 Q1 n1, R2 Q2 n2, R3 Q3 n3, L

Conclusions

Summary

Potentiostat setting

FRA setting

OCP?

Potentiostat or Galvanostat?

Fix DC potential (current) or potential

scan?

Potential scan

Potential Scan: Mott Schottky plot of a

semiconductor

of dopants.

Intercept gives Flat Band Potential

Frequency range?

Amplitude value?

Single sine or Multi sine?

1MHz -100mHz

10KHz -1mHz

Amplitude value?

Amplitude value?

50 mV = 42.1A

10 mV = 6.4A

Amplitude value?

100mV = 0.18A

200mV = 0.39A

Amplitude value?

Z=1 GOhm

10 mV leads to I=10 pA!!

Modern electrochemical

instrumentation and software allows

easy and fast data acquisition

Powerful data handling and analysis

tools are available

Data analysis remains a difficult task

measurement

or power supplies for high current or

high voltage measurements

DC current

IMPS and IMVS measurement on

photovoltaic device through modulation

of light intensity

DSC IMVS measurement at 625 nm,

OCP, E = 1.652 mW/cm2, DE = 10 %

DSSC charge transfer TiO2/dye/electrolyte

Diffusion process of I-/I3-

DSSC charge transfer TiO2/dye/electrolyte

Diffusion process of I-/I3-

Monitoring of impedance in

function of time

1800 seconds

Battery (LiPo)

! System knowledge is always required

! Impedance cannot be considered as a

stand alone

! Careful attention to the data

acquisition settings

Electrochemical impedance

spectroscopy one form of impedance

Rotation rate, mass, temperature,

light intensity, charge, etc

References

The reference handbook on impedance

spectroscopy

Spectroscopy: Theory, Experiment, and Applications,

Wiley-Interscience, 2005

References

Good reference book, specifically

focussed on Electrochemical

Impedance Spectroscopy

Impedance Spectroscopy, Wiley-Interscience, 2008

References

The reference handbook on

electrochemistry, also covers

impedance spectroscopy

Electrochemical Methods: Fundamentals and

Applications, Wiley, 2001

www.metrohm-autolab.com

All instruments covered by 3 years

factory warranty

Metrohm Autolab

Instruments for Electrochemistry

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