Cano, E. Electrochemical Protection System Mtal Artefacts. 2010
Letardi, P. y Cano, E. Electrochemical Protection Systems Metal Artefacts. 2010
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Transcript of Letardi, P. y Cano, E. Electrochemical Protection Systems Metal Artefacts. 2010
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ElectrochemistryinHistoricalandArchaeologicalConservation
WorkshopJan
uary11-152010
,Leiden,TheNetherlands
Electrochemical Assessment ofProtection Systems on Metal
Artefacts
P. LetardiCNR - ISMAR, Genoa, Italy
E.CanoCENIM-CSIC, Madrid, Spain
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ElectrochemistryinHistoricalandArchaeologicalConservation
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,Leiden,TheNetherlands
Introduction
Basic of EIS
Overview of commercially availableinstruments
Electrochemical cell and electrolyte
Data acquisition, representation andanalysis
Test of coatings for cultural heritage
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Basic of EIS
Energyleve
l(Potentia
lE)
Ref- - - -
Charge flow (Current I)
++ + +
The fundamental approach of
all impedance methods is to
apply a small amplitudesinusoidal excitation signal to
the system under investigation
and measure the response.
Theoretical Electrochemical
systems are usually
characterised by non-linear I-Ecurve .
A low amplitude sine wave
DEsin(wt), of a particular
frequency, is superimposed on
the dc polarization voltage E0.
This results in a currentresponse of a sine wave
DIsin(wt+f) superimposed on
the dc current I0. The current
response is shifted with
respect to the applied
potential.
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Basic of EIS
Perturbation: E(t)=E0 cos(w t) System response : I(t)=I0 cos(w t-f ) Response function: Z (w) = E/I
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Basic of EIS
Z(w) is a complex quantity with a magnitude and aphase shift which depends on the frequency of the
signal. Therefore by varying the frequency of the
applied signal one can get the impedance of the
system as a function of frequency.
Typically in electrochemistry, a frequency range of
100kHz 0.1Hz is used.
The plot of the real part of impedance on the X-axis
and the imaginary part on the Y-axis gives a
Nyquist Plot. While plotting data in the Nyquistformat the real axis must be equal to the imaginary
axis so as not to distort the shape of the curve. The
advantage of Nyquist representation is that it gives
a quick overview of the data and by the shape of
the curve one can make some qualitative
interpretations of the data. The disadvantage is that
one loses the frequency dimension of the data.
The absolute value of impedance (|Z|=Z0) and the
phase shifts are plotted on the Y-axis with log
frequency on the X-axis in two different plots giving
a Bode plot. This is the more complete way ofpresenting the data.
Zre
Zim
w0w
|Z|
Nyquist Plot|Z|
101
102
103
104
105
frequency [Hz]
10-2 10-1 100 101 102 103 104 105
-90
-60
-30
0
Bode Plot
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EIS spectrum can provide
information about
electrochemical processes...
and interface
properties
C.Gabrielli Identification of Electrochemical Processes by FrequencyResponse Analysis, (1998)
http://accessimpedance.iusi.bas.bg/vlab2/e-school/tech04.pdf
A.Amirudin, D.Thierry Application of electrochemical impedance
spectroscopy to study the degradation of polymer-coated metals,Prog. Org. Coat. 26 (1995) 1-28
The EIS technique(Electrochemical Impedance Spectroscopy)
Basic of EIS
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Basic of EIS
Electrochemical Impedance Spectroscopy (EIS): 1. Basic Principles
http://www.ecochemie.nl/download/content/Appl011.pdfElectrochemical Impedance Spectroscopy (EIS): 2. Experimental Setup
http://www.ecochemie.nl/download/content/Appl012.pdf
Basics of Electrochemical Impedance Spectroscopy
http://www.gamry.com/App_Notes/EIS_Primer/EIS_Primer_2007.pdf
Basics of Electrochemical Impedance Spectroscopy
http://new.ametek.com/content-manager/files/PAR/078.pdf
Electrochemical Impedance Measurements: Instruments and Techniques
http://new.ametek.com/content-manager/files/PAR/079c.pdf
http://www.solartronanalytical.com/Pages/Electrochemistry.htm
http://www.ecochemie.nl/download/content/Appl011.pdfhttp://www.ecochemie.nl/download/content/Appl012.pdfhttp://www.gamry.com/App_Notes/EIS_Primer/EIS_Primer_2007.pdfhttp://new.ametek.com/content-manager/files/PAR/078.pdfhttp://new.ametek.com/content-manager/files/PAR/079c.pdfhttp://new.ametek.com/content-manager/files/PAR/079c.pdfhttp://new.ametek.com/content-manager/files/PAR/079c.pdfhttp://new.ametek.com/content-manager/files/PAR/079c.pdfhttp://new.ametek.com/content-manager/files/PAR/078.pdfhttp://new.ametek.com/content-manager/files/PAR/078.pdfhttp://new.ametek.com/content-manager/files/PAR/078.pdfhttp://www.gamry.com/App_Notes/EIS_Primer/EIS_Primer_2007.pdfhttp://www.ecochemie.nl/download/content/Appl012.pdfhttp://www.ecochemie.nl/download/content/Appl011.pdf -
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Instruments and methods
E I
CEWE
Electrolyte
Potentiostat
FRA
REF
PersonalComputer
Commercially available instruments
Electrochemical cell and electrolyte
WE Working Electrode:
the electrode under investigation
CE Counter Electrode:
the electrode necessary to close the electrical circuit
REF Reference Electrode:
the electrode used to determine the potential of the
working electrode precisely
Electrolyte:
It ensures electrical conductivity between WE and CE
Potentiostat: it is used to fix the DC value and to
apply a sinusoidal perturbation over it
Frequency Response Analyzer (FRA): controls
the EIS scan and impedance evaluation
Acquisition Software: controls Potentiostat and
FRA, and store data file
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Electrochemical cell and electrolyte
3 electrodeflat plate cell
WE: coated metal
RE: Usually SCE orAg/AgCl
CE: platinum,
graphite orstainless steelmesh, wire or rod
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Electrochemical cell and electrolyte
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Electrochemical cell and electrolyte
Immersion cell
Testing of waxcoatings
C. Price et al , Proceedings of Metal 95,James&James, London (1997) 233-241
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Electrochemical cell and electrolyte
Immersion cell
Testing of oilcoatings
D. Hallam et al, Proceedings of Metal 04, NationalMuseum of Australia, Canberra (2004) 388-399
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Electrochemical cell and electrolyte
a contact probe setup
measurement method
has been developed to
make measurements on
art object also
CE
REF
Cloth soaked with mineral water
Contact
probe
WE
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ST Contact ProbeCE: Stainless Steel
AISI 316
REF: Stainless Steel
AISI 316
inserted in PTFE
= 1.5 cmA= 1.77 cm2
REF
CE
REF cable
CE cable
Letardi P., in: P.A.Vigato (Ed.), The Science of Art, Outdoor bronze protective coatings: characterisation by a new contact-probeElectrochemical Impedance measurements technique, Libreria Progetto di Padova, 2002, pp. 173-178
Instruments and methodsElectrochemical cell and electrolyte
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Electrochemical cell and electrolyte
Integrated cell+EIS electronics
E. Angelini et al, IEEE Transactions on Instrumentation and Measurement 55 (2006) 436-441
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Electrochemical cell and electrolyte
Electrolyte: as close as possible to thereal environment of the object orspecially aggressive towards demetal/coating
NaCl 0.1M
Harrison (0.35% (NH4)2SO4+0.05% NaCl)
Mineral water (Letardi)
K2SO4 0.25M (Hallam)
Acetic acid (Dowsett)
P. Letardi et al., Proceedings of Metal 98, James&James, London (2001) 303-308
D. Hallam et al, Proceedings of Metal 04, National Museum of Australia, Canberra (2004) 388-399M. Dowsett et al., Proceedings of Metal 07, Rijkmuseum Amsterdam (2007) 26-31
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Overview of commercially available instruments
http://www.ecochemie.nl/?pag=7
http://www.gamry.com/Products/Potentiostats.htm
http://www.princetonappliedresearch.com/products/potentiostats.cfm
http://www.solartronanalytical.com/Pages/Electrochemistry.htm
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Overview of commercially available instruments
Transportable instrumentation
Gamry FAS1 Femtostat
Portable instrumentation
Gamry Ref600
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Data acquisition and representation
Bode plot Nyquist plot
E. Cano, D. Lafuente, D.M. Bastidas, J. Solid State Electrochem. 14(2010) 381-391
Do not miss phase angle graph!
Same scale!
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Bode vs. Nyquist
C. Gabrieli, Use and Application of Electrochemical Impedance
Techniques TECHNICAL REPORT NUMBER 24. Solartron Analytical (1997)
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Data analysis
Physio-chemical model from first principles
Equivalent circuits (EC)
Evaluation of single parameters (|Z| at lowfrequency, C coating, etc.)
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Equivalent circuits
EC= analogues that reproduce theelectrical properties of our system
Pasive elements: resistors, capacitors,inductances, and other special elements(CPE, Warburg Impedance, etc.)
Many circuits can be used to model the
same data
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Equivalent circuits
Gamry Instruments (2007) Basics of electrochemical impedance spectroscopyhttp://www.gamry.com/App_Notes/EIS_Primer/EIS_Primer_2007.pdf
A good fitting does not mean you choosed a good model!
h b
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The basic EC
Intact coating
10-3
10-2
10-1
100
101
102
103
104
105
-90-80
-70
-60
-50-40
-30
-20-10
0
100
101
102
103
104
105
106
107
10810
910
10
(b)
PhaseAnglef
Frequency / Hz
(a)
ImpedandeModulus|Z|/cm
2
20 40 60 80 100
-20
-40
-60
-80
-100
-Z"
/Mcm
2
Z' / M cm2
h b
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The basic EC
Damaged coating
10-3
10-2
10-1
100
101
102
103
104
105
-90-80
-70
-60
-50-40
-30
-20-10
0
100
101
102
103
104
105
106
107
10810
910
10
(b)
PhaseAnglef
Frequency / Hz
(a)
ImpedandeModulus|Z|/cm
2
20 40 60 80 100
-20
-40
-60
-80
-100
-Z"/kcm
2
Z'/ k cm2
2 4
-2
-4
h b C
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The basic EC
Damaged coating(CPE)
20 40 60 80 100
-20
-40
-60
-80
-100
-Z"/kcm
2
Z'/ k cm2
2 4
-2
-4
10-3
10-2
10-1
100
101
102
103
104
105
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
100
101
102
103
104
105
106
107
108
109
1010
(b)
PhaseAnglef
Frequency / Hz
(a)
ImpedandeModulus
|Z|/cm
2
Th b i EC
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The basic EC
Damaged coating(CPE)
wjYZCPE
0
1
=1 CPE=C =0 CPE=R =-1 CPE=L =0.5 CPE=W
Usually, CPE is interpreted as an imperfect capacitor
Th b i EC
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The basic EC
Difussion(Warburg Imped.)
20 40 60 80 100
-20
-40
-60
-80
-100
-Z"/Mcm
2
Z'/ M cm2
10-3
10-2
10-1
100
101
102
103
104
105
-90
-80
-70
-60
-50
-40
-30
-20
-10
0
100
101
102
103
104
105
106107
108
109
1010
(b)
PhaseAnglef
Frequency / Hz
(a)
ImpedandeModulus
|Z|/cm
2
O h EC
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Other EC
Multiple paralel R-C
S-J. Lee and S-I Pyun, J Solid State Electrochem 11 (2007)829-839
O h EC
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Other EC
Multiple nested R-C
M. Evesque, M. Keddam and H. Takenouti, Electrochim.Acta 49 (2004) 2937-2943
Si l EIS t
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Single EIS parameters
|Z| max or |Z| low f C coat C
DL f min high f
EIS l i ft
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EIS analysis software
Zview (Scribner) EIS300 (Gamry)
PowerSine (PAR)
EIS SpectrumAnalyser (freeware!!!)
http://www.abc.chemistry.bsu.by/vi/analyser/
T t f ti f lt l h it
http://www.abc.chemistry.bsu.by/vi/analyser/http://www.abc.chemistry.bsu.by/vi/analyser/ -
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Test of coatings for cultural heritage
UN MN UA
Natural
80 years
urban
20 m
brochantite
|Z|10mHz = 69 18 K
Natural
1 year
marine
30 m
Atacamite|Z|10mHz = 5 2 K
Artificial
Pichler
process
80 m
brochantite|Z|10mHz = 29 4 KUrban artificial UA Substrate
Treatment
none Tref T1S T2S T3S
|Z| 10mHz
[K]
100
101
102
103
104
105
UA substrate
Urban Natural UN Substrate
Treatment
none Tref T1S T2S T3S I1S Iref
|Z| 10mHz
[K]
100
101
102
103
104
105
UN substrate
UN substate (1)
Marine natural MN Substrate
Treatment
none Tref T1S T2S T3S I1S Iref
|Z| 10mHz
[K]
100
101
102
103
104
105
MN substrate
Patina plays arelevant role
on coatingbehaviour
composition thickness texture
porosity
T t f ti f lt l h it
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Test of coatings for cultural heritage
[C]
[B
]
[D]
[A] [F]
[E]
[A] - Soter 201LC
[B] - R21
[C] - Tromm TeCe 3534F
[D] - Incralac
[E] - Incralac+Soter
[F] - Incralac+R21
Test on monuments could be prone to several limitations: accessibility
outdoor measurements
variables out of control
authorisations
T t f ti f lt l h it
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Test of coatings for cultural heritage
Test on monuments could be prone to several limitations:
previous restoration treatments are also to be considered carefully
Test of coatings for c lt ral heritage
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Test of coatings for cultural heritage
Coupons for testing:
alloy composition dimension
patina
natural (new)
natural (old)
artificial
characterisation
Coating application:
method thickness
characterisation
Test of coatings for cultural heritage
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Test of coatings for cultural heritage
wheatering:
Multiple coupons for statistical reasons
naturalEN ISO 8565 Metals and alloys Atmospheric
corrosion testingGeneral requirements for field
tests.
artificialEN ISO 11341 - Paints and varnishes. Artificial
weathering and exposure to artificial radiation.
Exposure to filtered xenon-arc radiation
EN ISO 9227 - Corrosion tests in artificial
atmospheres. Salt spray tests
Test of coatings for cultural heritage
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Test of coatings for cultural heritage
Because of the large number of variables
involved, one need several coupons in order
to check the behaviour
Statistical methods such as Experimental
Design could be of great help in order toreduce the number of experiments required
http://www.itl.nist.gov/div898/handbook/pri/section3/pri3.htm
http://www.chemometrics.se/images/stories/pdf/aug2002.pdf
J. A. Bishopp, M. J. Parker and T. A. OReilly, The use of statistical experimental design procedures in
the development and robust manufacture of a water-based, corrosion-inhibiting adhesive primer,
International Journal of Adhesion and Adhesives 21,(2001), 473-480M.J. Anderson, P.J. Whitcomb, Design of experiments for coatings, in A.A. Tracton, Coatings
Technology Handbook, Third Edition, 3rd ed., CRC Press, 2005
Further references
http://www.itl.nist.gov/div898/handbook/pri/section3/pri3.htmhttp://www.chemometrics.se/images/stories/pdf/aug2002.pdfhttp://www.chemometrics.se/images/stories/pdf/aug2002.pdfhttp://www.itl.nist.gov/div898/handbook/pri/section3/pri3.htm -
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Further references
Cano E, Bastidas DM, Argyropoulos V, Fajardo S, Siatou A, Bastidas JM, Degrigny C (2009)Electrochemical characterization of organic coatings for protection of historic steel artefacts. Journal of
Solid State Electrochemistry, 1-11.
Cano E, Lafuente D, Bastidas DM (2009) Use of EIS for the evaluation of the protective properties ofcoatings for metallic cultural heritage: a review. Journal of Solid State Electrochemistry, 1-11.
Loveday D, Peterson P, Rodgers B (2004) Evaluation of organic coatings with electrochemicalimpedance spectroscopy: Part 1: Fundamentals of electrochemical impedance spectroscopy. JCTCoatingsTech1, 46-52.
Loveday D, Peterson P, Rodgers B (2005) Evaluation of organic coatings with electrochemicalimpedance spectroscopy. JCT CoatingsTech2, 22-27.
Loveday D, Peterspm P, Rodgers B (2004) Evalution of organic coatings with electrochemicalimpedance spectroscopy part 2: Application of EIS to coatings. JCT CoatingsTech1, 88-93.
Mansfeld F (1995) Use of electrochemical impedance spectroscopy for the study of corrosion protectionby polymer coatings. Journal of Applied Electrochemistry25, 187-202.
Letardi P., Laboratory and field test on patinas and protective coating systems for outdoor bronzemonuments, in: Ashton J., Hallam D.(Eds.), Proceedings of Metal2004, National Museum of Australia,Canberra, 2004, pp. 379-387
Joseph E., Letardi P., Mazzeo R., Prati S., Vandini M., Innovative treatments for the protection ofoutdoor bronze monuments, in: C.Degrigny, R. van Langh, I. Joosten, B.Ankersmit (Eds.), Proceedingsof Metal07, Amsterdam 2007, v5 pp. 71-77