Tiêu chuẩn iso 16773 3 2016

© ISO 2016 Electrochemical impedance spectroscopy (EIS) on coated and uncoated metallic specimens — Part 3 Processing and analysis of data from dummy cells Spectroscopie d’impédance électrochimique (S[.]

Electrochemical impedanc e

Part 3:

Proc essing and anal ysis ofdata from

S ec trosco ie d’imp da c électrochimique (SIE) sur de s é ro vete s

métalique s r vê tue s et n n r vê tue s —

Partie 3: Traitement et a alyse des do n e s o ten es à p rtir de

ce llule s test

S con edition

2 16-04-0

Refer ence n mb r

ISO 16 73-3:2 16(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2016, P blshed in Sw itz rlan

A ll rig hts r eserved Unles otherw ise spe ified, nopar of this p blc tion ma y be r epr od c d or utilz d otherw ise in an form

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written permis ion Permis ion c n be req esed from either ISO at the ad r es below or ISO’s member bod y in the c u try of

the r eq eser

ISO c pyrig ht ofic

C de Blan on et 8 • C 4 1

CH-1 14 Vernier, Geneva, Sw itzerlan

F reword i v

1 Sc ope 1

2 Des riptio of the d mmy c els 1

2.1 General 1

2.2 Comp nent of the d mmy c ls 1

2.3 A ccuracy r eq ir ements for the components 2

2.4 Cir cuit desc iption 2

3 Proc ed re .3

4 Data anal ysis 3

5 Presentatio of the results 3

6 Ac c eptanc e c iteria for the me sur ement system 5

7 Test rep rt 5

8 Repe tabiity and r eproducibiity 6

Biblog raphy 11

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b dies (ISO membe b dies) The work of pr p ring Int ernational Stan ards is normaly car ied out

through ISO t ech ical committ ees Each membe b dy int er st ed in a subje t for w hich a t ech ical

committ ee has be n es a lshed has the right t o be r pr sent ed on that committ ee Int ernational

org nizations, g ove nmental an non-g ove nmental, in laison with ISO, also take part in the work

ISO cola orat es closely with the Int ernational Ele trot ech ical C mmis ion (IEC) on al matt ers of

ele trot ech ical s an ardization

The proc d r s used t o develo this document an those int en ed for it furthe maint enanc ar

desc ibed in the ISO/IEC Dir ctives, Part 1 In p rticular the dife ent a pro al c it eria ne ded for the

dife ent ty es of ISO document should be not ed This document was draft ed in ac ordanc with the

edit orial rules of the ISO/IEC Dir ctives, Part 2 ( e www.iso.org dir ctives)

A tt ention is drawn t o the p s ibi ity that some of the element of this document ma be the subje t of

p t ent right ISO shal not be held r sp nsible for identifying any or al such p t ent right Detais of

any p t ent right identified d ring the develo ment of the document wi be in the Introd ction an / r

on the ISO ls of p t ent de larations r c ived ( e www.iso.org p t ent )

Any trade name used in this document is information given for the convenienc of use s an does not

cons itut e an en orsement

F or an ex lanation on the meaning of ISO spe ific t erms an ex r s ions r lat ed t o conformity

as es ment, as wel as information a out ISO’ s adhe enc t o the WTO principles in the Te h ical

Bar ie s t o Trade (TBT) se the fol owing URL: F or word - Sup lementary information

The committ ee r sp nsible for this document is ISO/TC 3 , Paint a d v rni shes , Subcommitt ee SC 9,

G ene al tes t meth ds fr p ints a d v rni shes

This se on edition canc ls an r plac s the f irs edition (ISO 1 7 3-3:2 0 ), w hich has be n

t ech icaly r vised The main chang es ar the folowing:

a) the introd ct ory element of the title, Paints a d v rni shes , has be n omitt ed, be ause the sco e

is bro dened t o inclu e metals an aloy s an the main element of the title has be n chang ed t o:

Elec trochemic al impeda c e s pec tros c op (EIS) o c oated a d u c oated metal c s pec imens;

b) a r fe enc t o ISO/TR 1 2 8 for d mmy c ls with low impedanc v lues (1 Ω t o 1 0 0 Ω) has

be n ad ed;

c) a r fe enc t o ASTM G 10 for the pr cision data of low impedanc measur ment has be n ad ed;

d) a t es r p rt has be n ad ed

ISO 1 7 3 consis s of the folowing p rt , u de the g ene al title Elec trochemic al impeda c e s pec trosc op

(EIS) o c oated a d u c oated metal c s pec imens:

— Part 1: Te ms a d de initio s

— Part 2 : Colec tio o data

— Part 3 : Proces s in a d a alys i s o data from dummy c ell s

— Part 4 : Ex mples o s pec tra o p ly me -c oated a d u c oated s pec imens

Electrochemical impedanc e spectrosc opy (EIS) on c oated

Part 3:

This p rt of ISO 1 7 3 spe ifies a proc d r for the ev luation of the ex e imental set-up used for

car ying out EIS on high-impedanc co t ed samples F or this purp se, d mmy c ls ar used t o simulat e

high-impedanc co t ed samples On the b sisof the eq iv lent cir uit desc ibed, this p rt of ISO 1 7 3

gives guidelnes for the use of d mmy c l s t o inc ease conf idenc in the t es prot ocol, inclu ing making

measur ment , curve f it ing an data pr sentation

NOTE Due t o the nature of the me surements, investig tions of high-mpedance co ted samples are more

sus eptible t o artefacts coming from electroma netic interferences T erefore, this part of ISO 16 73 consider

the aspects for me suring high-mpedance samples by using ap ropriat e d mmy cel s in a F araday ca e.However,

most man facturer ofer complementary d mmy cels in the low an medium impedance rang T is alows

checking the setu in the respective low impedance rang

2 Desc iption of the dummy c el s

2.1 General

A set of four eq iv lent cir uit (d mmy c l s) is used t o che k the o e al ex e imental ar ang ement

The d mmy c l s ar mou t ed sep rat ely Two ty es of eq iv lent cir uit, A an B, ar used, as shown

in Figur 1 The spe if ic ele trical comp nent of these four c ls ar given in Ta le 1 Dummy c ls with

low impedanc v lues (1 Ω t o 1 0 0 Ω) ar desc ibed in ISO/TR 1 2 8

NOTE In Clause 8, the results of an int erla orat ory test are used t o evaluat e the precision of this method

During the int erla orat ory test, the participating la orat ories also me sured a f if h d mmy cel consisting of an

eq ivalent cir uit of ty e Bwith u k own component values

2.2 Components ofthe dummy c el s

Each d mmy c l consis s of a combination of r sist ors an ca acit ors w hich ar solde ed dir ctly ont o

a print ed-cir uit b ard ( e Figur s 1 and 2) Such networks of r sist ors an ca acit ors (eq iv lent

cir uit ) ar oft en used in work on high-impedanc co t ed spe imens

NOTE Because of the very high overal resistance of cir uits A an B, the resist or simulating the electrolyt e

can b ne lect ed T picaly, the values of resistances R

1

an R

2 are a ove 1 0 MΩ where s the electrolyt e

resistance is arou d 1 0Ω t o 5 0 Ω As a conseq ence, the electrolyte resistance is not signif icant in this kin of

EIS ap lication

The v lues of the component of the four d mmy c l s ar chosen in ac ordanc with the folowing

conside ations

— Dummy c l 1should che k the input r sis anc aswel as the input ca acitanc of themeasur ment

eq ipment

— Dummy c l s 2 t o 4 should che k the ca a i ty of the ev luation sof war an the impedanc

measur ment eq ipment t o dis inguish betwe n only sl ghtly dife ent r sist or/ca acit or

combinations

Figure 1 — E uivalent cir uits of the dummy cel s

Table 1 — Values of the compo ents of the dummy cel s

Dummy c l Cir uit

R

1

GΩ

R

2

GΩ

C

1

n

C

2

n

2.3 Ac curacy r equirements for the c omponents

The ac uracy r q ir d for r sist ors below 1

9

Ω is ±2 % an for r sist ors a o e 1

9

Ω it is ±5 % The

ac uracy r q ir d for the ca acit ors is ± % Such r sist ors an ca acit ors ar a ai a le comme cialy

2.4 Cir cuit des r iption

Usualy, the measur ment of high-impedanc co tings r q ir s only a two-ele trode set-up, but

ele trochemical works ations ofe the pos ibi ity of conne ting up thr e or four ele trodes To

simplfy the conne tion of the d mmy c l s t o ele trochemical works ations, each c l should ha e

four conne t ors (as in icat ed in Figur 2), the con e t ors being con e t ed int ernaly in p irs To a oid

contamination (e.g b fing erprint ) of the print ed-cir uit b ard, each d mmy c l is prot ect ed b

ac y lic plat es mount ed on t op of an u de neath the c l

Key

1, 2 con ector pair

Figure 2 — Photograp of a d mmy cel used in the inter laboratory test

3 Procedure

Pe form al measur ment in a F arada cag e in orde t o minimiz ele troma netic int erfe enc

NOTE T e four d mmy cels alow the suita ility of a shielding t ech iq e (i.e a F araday cag e) t o b

det ermined, as wel as helping t o f in the location in the la orat ory where electroma netic noise levels are lowest

Pe form the measur ment in ac ordanc with the man factur r’s r commen ations in the

p t entios atic mode at a DC v lue of z ro v lt , using an ampltu e of 2 mV (peak-t o-z ro)

A fr q ency rang e betwe n 1

4

Hz an 1

−

Hz is suff icient for measur ment with d mmy c l s 2 t o

4 F or d mmy c l 1, a fr q ency rang e of 1 0 0 Hz t o 5 × 1

−

Hz is r commen ed Ab ut 3 min t o

40 min ar r q ir d for a single measur ment (for d mmy c l 1, a out 1 h)

If the r sult of the measur ment ar not satis act ory w hen using an ampltu e of 2 mV, inc ease the

ampl tu e

4 Data anal ysis

Using suita le sof war , e.g that sup led b the man factur r of the ele trochemical works ation,

analy se the r sult o tained from the d mmy c l with eq iv lent cir uit A ( e Ta le 1) R ecord the

r sult of curve fit ing, the theor tical v lues of the cir uit comp nent an the ex citation p t ential

w hich was a pled

NOTE 1 Unfortu at ely, the curve-f it ing er or given for the data analy sed difer from man facturer to

man facturer, so direct comparison is not pos ible

Pr p r a Bode plot with the measur d an simulat ed data

NOTE 2 Although the curve-f it ing er or are not compara le, the Bode plot gives an in ication of the q ality

of the me sured data, especialy at low freq encies

R epeat the analy sis with the r sult from c ls 2 t o 4 using eq iv lent cir uit B ( e Ta le 1)

5 Presentation of the results

Pr sent the measur d data as Bodeplot for comp rison purp ses

The Bode plot in Figur 3 show how the d mmy-c l measur ment should lo k These dia rams

we e calculat ed using simulation sof war an can be used t o compar with r sult from d mmy-c l

measur ment

1

2

Y

Y

1

1

9

8

7

6

9

75

60

45

3

1

a)Cel 1

1

Y

2

1

2

60 9

6 7 8 9 1

b) Cel 2

1

2

Y

2 Y

1

9

75

60

7 8 9

c) Cel 3

Y

1

2

9

2

1 Y

4 5

7 8

d) Cel 4

2

Y

Y

1

2

4

7 8 9

1

9

e)Cel 5 (values of compo ents unknown)

Key

X log f(fin Hz)

Y

1

log |Z|(Z in Ω)

Y

2

|φ|(deg r ees)

1 p ase angle φ

2 impedance Z

Figure 3 — Bo e plots of the simulated impedance spectra of the d mmy cel s and the

unkn wn cel

6 Ac c eptanc e c iteria for the measur ement system

The EIS sys em shal be ca a le of measuring and extracting the v lues of the r sist ors an ca acitors

in the d mmy c ls Deviations of the f it ed v lues of the ele tronic comp nent from the r al v lues

( e Ta le 1) should not ex ce d the ac uracy l mit of the comp nent used in the d mmy c l s

Exc s ive e rors in the v lues in icate ex e imental pro lems with the EIS sys em or inac urate

o e ation of the sys em

NOTE Guidance is given in ISO 16 73-2

7 Test r eport

If a t es r p rt is r q ir d for the documentation of d mmy-c l measur ment , it hal contain at leas

the folowing information:

a) al detais ne es ary t o identify the d mmy c l t est ed an it ac uracy of ele tronic comp nent ;

b) a r fe enc t o this p rt of ISO 1 7 3, i.e ISO 1 77 -3;

c) the t empe atur an r lative h midity d ring the con itioning an t es , if dife ent from those

spe ified in ISO 1 7 3- 2: 2 1 , 6.7.2;

d) thet es method used inclu ing ex citation con itions an t es d ration, in p rticular:

1) fr q ency rang e, an

2) ampltu e;

e) the r sult o tained from fit ing of the r spe tive eq iv lent cir uit t o the measur d data, as

in icat ed in Cla use 4;

f) any deviations from the proc d r spe ified;

g) any u usual featur s (anomales)o se ved d ring the t est ;

h) thedat e of the t es

8 Repeatabi ity and reproducibi ity

F or the det ermination of the pr cision data of high impedanc measur ment , an int erla orat ory t es

was car ied out, detai s se below F or the pr cision data of low impedanc measur ment , r fe t o

ASTM G 10

F ourt een la orat ories, mainly in E ro e an the USA, p rticipat ed in an int erla orat ory t es The

purp se of the int erla orat ory t es was t o o tain an es imat e of the r peata i ity an r prod cibi ty of

the proc d r Each la orat ory made measur ment with thefour d mmy c l s ( e Ta le1)an with a

fifh c l (cir uit B) with un nown comp nent Aft er measur ment and curve fit ing, the r sult we e

as shown in Ta les 2 t o 6

In cases w he e the measur ment we e ac epta le ( e Clause 6), it was foun that the r peata i ty

w as ve y g ood, the deviations betwe n measur ment being bett er than the ac uracy of the cir uit

comp nent

The r prod cibi ity of the measur ment made with c l s 1 t o 5 can be es imat ed from Ta les 2 t o 6

1)

It can be se n that not eve y la orat ory was a le t o make measur ment with c l 1 with suff icient

ac uracy Cel 2 g ve no pro lemsfor any of the la orat ories Cel s 3 an 4 we e mor difficult for some

la orat ories, although the majority we e a le t o measur the cor e t v lues

Table 2 — Reprod cibi ity of me surements with cel 1

L b rat ory

R

GΩ

C

p

Ampl tu e

mV

Er or in R

%

Er or in C

%

Total e ror

%

a

N.A

a

a

N.A

a

N.A a

Stan ard

deviation

a

N.A = Not avaiable

Table 3 — Reprod cibi ity of me surements with cel 2

L b rat ory

R

1

C

1

R

2

C

2 Ampl

-tu e

Er or

in R

1

Er or

in C

1 Total

e ror

Er or

in R

2

Er or

in C

2 Total

e ror

Stan ard

deviation

Table 4 — Reprod cibi ity of me surements with cel 3

L b rat ory

R

1 C

1 R

2 C

2 Ampl

-tu e

Er or

in R

1

Er or

in C

1 Total

e ror

Er or

in R

2

Er or

in C

2 Total

e ror

Me n value 1,57 0,1 0,34 2 ,3

Stan ard

deviation

Table 5 — Reprod cibi ity of me surements with cel 4

L b rat ory

R

1 C

1

R

2

C

2 Ampl

-tu e

Er or

in R

1

Er or

in C

1 Total

e ror

Er or

in R

2

Er or

in C

2 Total

e ror

a

N.A

a

N.A

a

N.A

a

a

N.A

a

N.A

a

N.A

a

N.A

a

N.A a

Stan ard

deviation

a

N.A = Not avaiable

Table 6 — Repro ucibi ity of me surements with cel 5 (values of components unknown)

L b rat ory

R

1 C

1 R

2 C

2 Ampl

tu e

Er or

in R

1

Er or

in C

1 Total

e ror

Er or

in R

2

Er or

in C

2 Total

e ror

Stan ard

deviation

The v lues for c l 5 ar the folowing:

R

1

= 5 GΩ

C

1

= 0,1 nF

R

2

= 7,5 GΩ

C

2

=0,42 nF

Cel 5wasfitt ed with comp nent w hich had v lues un nown t o the p rticip nt and it urned out that

the pr cision was significantly worse than with the othe c l s ( e Figur 4)