Tiêu chuẩn iso 20343 2017

© ISO 2017 Fine ceramics (advanced ceramics, advanced technical ceramics) — Test method for determining elastic modulus of thick ceramic coatings at elevated temperature Céramiques techniques — Méthod[.]

Fine c eramics (ad vanc ed c eramics,

Céramique s te h ique s — Méth de d’essai re lative à la déte mination

du module élastique de s r vê tement de céramique é ais à

temp ratur élev e

Fir t edition

2 17-0

Refer ence n mb r

ISO 2 343:2 17(E)

COPYRIGHT PROTECTED DOCUMENT

© ISO 2017, P blshed in Sw itz rlan

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F reword i v

1 Sc ope 1

2 Nor mati ve r eferenc es 1

3 Terms an definitions 1

4 Principle 2

5 A pparatus 2

5.1 Elastic mod lus tes ing machine 2

5.2 Heating sys em 2

5.2.1 General 2

5.2.2 Temperatur e s a i ty 2

5.2.3 Tes temperatur e u iformity 2

5.2.4 Furnac heating rate 2

5.2.5 Furnac s a i ty 2

5.3 Temperatur e measuring an indicating ins rument 2

5.3.1 General 2

5.3.2 The mocouples 3

5.3.3 Ve ification of the the mocouple temperatur e measuring sys em 3

5.4 Dimension-measuring devic 3

5.5 Tes fixture 3

5.5.1 General 3

5.5.2 Fix ture mate ial 3

6 Test piec es 3

6.1 Tes pie e siz 3

6.2 Tes pie e prep r ation and s orag e 4

7 Test pr oc edure 4

7.1 Measur ement of the siz an mas of the tes -pie es 4

7.2 Measur ement of elastic mod lus of co ting at elev ted temper atur e 4

8 Calculation of results 6

8.1 Stan ar d formula for elas ic mod lusof co ting 6

8.2 Mean v lue an stan ar d deviation for elas ic mod lus 6

8.3 Variation of elas ic mod lus with temper atur e 7

9 A nal ysis of pr ecisio and unc er tainty 8

10 Test rep r t 8

Biblog raphy 9

ISO (he Int ernational Org nization for Stan ardization) is a worldwidefede ation of national s an ards

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 sponsible 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

For an ex lanation on the meaning of ISO spe ific t erms an ex r s ions r lated to conformity as es ment,

as wel as information a out ISO’s adhe enc to the Wor ld Trade Org nization (WTO) principles in the

Te h ical Bar ie s to Trade (TBT) se the folowing URL: www.iso.org/ iso/for word.html

This document was pr p r d b Te h ical Committ ee ISO/TC 2 6, Fine c eramic s

Fine c eramics (ad vanc ed c eramics, ad vanc ed technical

This document spe ifies a method of t es for det ermining the elas ic mod lus of thick c ramic

monola e co tings ( hick es > 0,0 mm) at elev t ed t empe atur s, using the impulse ex citation

method Proc d r s for t es pie e pr p ration, t es modes an rat es (lo d rat e or displac ment), data

cole tion, an r p rting proc d r sar given

This document a ples primari y t o brit le c ramic co tings on c ramic or metal subs rat es This

t es method can be used for mat erial r sear h, q alty control, an charact erization an design

data-g ene ation purp ses

2 Normati ve r eferences

The folowing document ar r fe r d t o in the t ext in such a wa that some or al of their cont ent

cons itut es r q ir ment of this document F or dat ed r fe enc s, only the edition cit ed a ples F or

un at ed r fe enc s, the lat es edition of the r fe enc d document ( inclu ing any amen ment ) a ples

ISO 36 11, G eometric al produc t s pec ific atio s (GPS) — Dimens io al meas urin eq ipment: Mic romete s fr

ex te n l meas ur ment — Des ig a d metrolo ic al ch rac te i s tic s

ISO 1 561, Fine c eramic s (adva c ed c eramic s , adva c ed technic al c eramic s) — Tes t meth d fr elas tic

modul o mo olthic c eramic s at ro m tempe atur b s onic r s on nc e

IEC 6 5 4-1, Thermoc ou les — Part 1: EMFs pec ific ations a d tole a c es

3 Terms and definitions

F or the purposes of this document, the folowing t ermsand definitions a ply

ISO an IEC maintain t erminolo ical data ases for use in s an ardization at the folowing ad r s es:

— IECEle tro edia: a aia le at ht p:/ www.ele tro edia.org

— ISO Onlne brow sing plat orm:a ai a le at ht p:/ www.iso.org o p

3.1

elastic mo ulus

ratio of plane s r s t o plane s rain

Note 1t o entry: Also k own as You g’ s mod lus

3.2

flexural vibrations

vibrations that oc ur w hen the displac ment in a slen e rod or b r ar in a plane normal t o the length

dimension

3.3

thicknes ratio

ratio of the co ting thick es t o the subs rat e thick es

4 Principle

The elev t ed t empe atur elas ic mod lus of c ramic co tings on metal or c ramic subs rat es is

ded c d b comp ring the elas ic mod l of co t ed and u co t ed samples, un e the pr con ition that

the int erfac betwe n the co ting and the subs rat e is contin ous an without a deb n ing zone The

elas ic mod lus of c ramic co tings can be calculat ed from thr e p ramet ers, i.e the elas ic mod lus

of the u co t ed sample or subs rat e ( E

s , eq iv lent elas ic mod lus of the co t ed sample ( E

q ), an the

ratio of the co ting thick es t o thesubs rat e thick es ( R = h/H) The v lue of E

q

an E

s

ar det ermined

b the impulse ex citation t echniq e

5.1 Elastic modulus testing machine

A suita le impulse ex citation t es ing syst em ca a le of a plying impulses at elev t ed t empe atur s

shal be used, w hich shal be in ac ordanc with ISO 1 56 1 Sinc the t es pie e is r q ir d b ISO 1 561

t o be homog eneous and isotro ic, the measur d mod lus using the co t ed t es pie e is then desc ibed

as an eq iv lent elas ic mod lus

5.2 He ting system

5.2.1 General

The heating sy st em, usual y a furnac , shal be ca a le of heating the t es fixtur an t es pie e an

maintaining a u iform an cons ant t empe atur d ring the impulse ex citation t es The furnac shal

ha e the ca a i ty for containing air, ine t g s, or a v cu m environment as r q ir d for the t es

5.2.2 Temperature stabiity

The furnac shal be controled b a devic ca a le of maintaining a cons ant t empe atur within ± °C

or bett er within it working spac d ring the time w hen the elas ic modulus of t es pie es is being

measur d

5.2.3 Test temperature unifor mity

The furnac shal be ca a le of maintaining a u iform t es pie e t empe atur It shal pr viously

be det ermined that the t empe atur of the t es pie e does not v ry b mor than 0,5 % of the t es

t empe atur aft er a 1 min hold time at the r q ir d t es t empe atur measur d in °C

5.2.4 F rnac e he ting rate

The furnac control devic shal be ca a le of maintaining a heating rat e of the furnac of 5 °C min t o

1 °C min and pr venting t empe atur o e sho t

5.2.5 F rnac e stabiity

The time for the sy st em t o r ach the mal eq i brium at the t es t empe atur shal be det ermined for

the t es t empe atur t o be used

5.3 Temperatur e measur ing and indicating instr uments

5.3.1 General

The the mocouple t empe atur measuring eq ipment shal ha e a r solution of at leas 1 °C an an

ac uracy of 5 °C or bett er Optical pyromet ers, if used, shal ha e a r solution of bett er than 5 °C an an

ac uracy of 5 °C or bett er

5.3.2 Ther moc ouples

The mocouples in ac ordanc with IEC 6 5 4-1 shal be used The the mocouple shal exhibit

low the mal ine tia ( he diamet er of the wir s shal not be gr at er than 0,5 mm) The measuring

the mocouple tip shal be les than 2 mm from thet es pie e, but neve contact the t es pie e

5.3.3 Ver ificatio of the ther moc ouple temperature me sur ing system

The mocouples shal be calbrat ed pe iodicaly a ains national s andards sinc calbration ma drif

with usag e or contamination

5.4 Dimension-me suring devic e

A Ve nie cal pe with a pr cision of 0,0 mm ac ording t o ISO 3611 should be used t o measur the

dimensions of the t es pie e The thicknes ofthe co ting shal be measur d b using a trac a ly

calbrat ed o tical or scanning ele tron mic osco e ( SEM)with ma nif ication of1 0 0 times or bett er

5.5 Test fix ture

5.5.1 General

The f ixtur shal be suita le for the ins alation of the t es pie e as r commen ed in ISO 1 56 1 with

platin m hanging wir s an for impulse ex citation an signal acq isition in the furnac The fixtur

shal maintain the p sition of the t es pie e d ring the t es

5.5.2 Fix ture material

The f ixtur shal be man factur d from a mat erial that is ine t u de the t es ing con itions used The

fixtur shal be o idation-r sis ant if the t es ing is con uct ed in air The f ixtur shal ha e neglgible

chemical r action with an shal not contaminat e the t es pie e

6 Test piec es

6.1 Test piec e size

A r ctangular t es b r with co ting on one of the two larg es fac s only is r q ir d The g eometrical

dimensions of the co t ed sample ar displayed in Figur 1 The thick es ratio, R ( R = h/H), shal

be larg er than 1/ 10 F or flexural r sonanc , the length of the spe imen ( L) shal be gr at er than

40 mm The ratio of length t o thick es of subs rat e, L /H, shal be gr at er than 2 The ratio of width

t o thick es of subs rat e, B/H, shal be in the rang e of 3 t o 1 The p ralelsm t ole anc on o p sit e

longitu inal fac s is 0,0 5 mm Ta le 1 show s the r commen ed dimensions of a c ramic -co t ed t es

pie e Thesurfac ofthe t es pie e shal be smo th an flat The surfac shal be grou d using a f ine grit

(40 grit or f ine ) Any machining proc d r used shal not afe t he r sult The edg esofthe t es pie e

shal not be chamfe ed

Key

1 co ting

2 substrate

Figure 1 — Schematic i lustratio of the rectangula test pieces

Table 1 — Recommended dimensio s for coated test piece

Dimensions in milimetr es

An ap ro imate ratio for L:B:( H + h) = 20:5:1 is re ommen ed for elas ic mod lus me surement of thick c ramic c atin

with h > 0,03mm an 1> h/ H > 0,01

6.2 Test piec e pr eparation and storag e

The t es pie es ma be o tained using one of the two a pro ches

a) The t es pie es ar cut from some co t ed comp nent , car fuly grin ing and pol shing the t es

pie e t o ke p the surfac s paral el an flat

b) The t es pie esar pr p r d b co ting a subs rat e;in this case, the mod lus of the subs rat e shal

be measur d befor depositing the co ting The detaied t es proc d r is desc ibed below Befor

a plying the co ting, mark each t es pie e subs rat e with a uniq e identif ie w hich wi be visible

aft er co ting Measur the flatnes of each u co t ed t es pie e, for ex mple, b mou ting in an

uns r s ed s at e on the x-y s ag e of a calbrat ed o tical mic osco e an measuring the z co rdinat e

of the surfac with an ac uracy of ± µm at 1 eq al y sp c d positions along it length R ecord the

r sult for each t es pie e

The t es pie es shal be han led car fuly t o a oid the introd ction of damag e aft er t es pie e

pr p ration The t es pie esshal be st or d sep rat ely an not alowed t o imp ct or sc at ch each othe

A minimum of 5 t es pie es is r q ir d for the t es

7 Test pr oc edur e

7.1 Measurement of the size and mas of the test-pieces

Dry the t es pie es unti their mas is cons ant Weigh each of the t es pie es t o the near s 1 mg or

0,1 % (w hicheve is gr at er) using a calbrat e scale Measur the length of co t ed t es pie e t o the

near s 0,0 mm or 0,1 % (w hicheve isgr at er) Measur the thick es of co ting an the subs rat e t o

near s 0,0 1 mm or 0,1 % (w hicheve is gr at er)

Measur the dimensions of the t es pie es using a Ve nie cal pe complying with ISO 36 11 an with

pr cision of 0,0 mm or bett er, or othe calbrat ed measuring devic pro iding the same or bett er

measur ment ac uracy Measur the width an thick es at thr e p int along it length ac ording

t o 5.5 (at the mid le an two ends of the b r) an det ermine the a e ag e of the thr e measur ment

Co ting thick es shal be measur d b using a cal brat ed o tical or scan ing ele tron mic osco e

( SEM) with ma nification of 1 00 times or bett er

The v riation in co ting thick es betwe n the thickes an thin es v lues measur d shal be les than

or eq al t o 1 % If the v riation is mor than this, pr p r new t es pie es me ting this r q ir ment

Car ne ds t o be taken with the pr p ration of the side of the sample so that g ood contras is o tained

betwe n the co ting an subs rat e so that g ood measur ment of co ting thick es can beo tained

7.2 Measurement of elastic modulus of coating at elevated temperature

Suspen one of the t es pie es, sup ort ed b a heat-r sis ing mat erial lke platin m wir in ac ordanc

with ISO 1 56 1, as shown in Figur 2, in the furnac The suspen ing devic s shal pe mit the fr e

vibration of the t es pie e The elas ic mod lus of the subs rat e shal be k own, or be measur d at the

t empe atur or t empe atur s of int er s , using an u co t ed sample

a) Impulse ex citatio testing metho

b) Recommended support sy stem

Key

1 su port system

2 imp lser

3 furnace

4 specimen

5 tr ansd cer

6 sig nal amplifier

7 fr eq ency analyzer

8 results outp t

Figure 2 — Schematic ilustratio of impulse excitatio testing meth d and recommended

support sy stem

Heat the t es pie e t o the t es ing t empe atur an hold it at this t empe atur for a suff icient time (1 min

is r commen ed) for the spe imen t empe atur t o r ach eq i ibrium The time alowed for thisshal be

s at ed in the t es r p rt The t empe atur measur d b the the mocouple or othe measuring devic

shal not v ry d ring the time of the t es ing b mor than ±0,5 % of the t es t empe atur measur d in

°C Ex cit e flexural r sonanc of the samples b a plying an impulse an measur the fr q ency of the

r sonanc g ene at ed Det ermine the elas ic mod lus of subs rat e, E

s , an the elas ic mod lus of co t ed

t es pie es, E

q

, ac ording t o ISO 1 561, r spe tively Tes r sult shal be o tained from at leas 5 co t ed

t es pie es, al of w hich wer co t ed at the same time b the same proc s

8 Calculation of r esults

8.1 Standard formula for elastic modulus of coating

The s an ard formula for the elas ic mod lus of the co ting, E

c , is given b F ormula (1):

E

R

E

=

⋅ 2

3

2

(1)

w he e

F=(1+R) ⋅(E /E )

3

(3)

A=4R +6R+4−F

2

(4 )

C=4R ⋅ F−1

2

w he e

h is the thicknes of c ramic co ting, in mm;

H is the thicknes of the subs rat e, in mm;

E

q

is the elas ic mod lusof co t ed spe imen, in GPa;

E

s

is the elas ic mod lusof subs rat e, in GPa

Det ermine the thick es ratio, R, using F ormula (2) an the s ifnes ratio of the subs rat e sample t o the

co t ed sample, F, using F ormula (3) Calculat e the v lues of A an C using F ormula (4 ) an F ormula (5),

r spe tively The elas ic mod lus of the co ting, E

c , can then be o tained using F ormula (1)

Th s, the t es proc d r for co ting’s mod lus has thr e st eps

a) Measur the mod lus of co t ed t es pie e v rying with t empe atur

b) Tes the mod lus of the subs rat e v rying with t empe atur

c) C lculat e the mod lus of the co ting at dife ent t empe atur s

8.2 Mean value and standar d deviation for elastic modulus

The mean elas ic mod lus, E, an the s an ard deviation, s , ar given b F ormula (6) an F ormula (7):