KR0100936

KAERI/RR-2077/2000

til-

Materials Characterization by Resonant Ultrasonic

Spectroscopy

3 2 / 48

2001. 1.

;§ -g-

A] ^ JS.

- 1 -

A £

II.

Q-factor

ffl. ^ ^ 7 f l « ^ ufl-g-

- 11 -

iv.

^ ^ r 7fi >£*}&_&

RMS error7} 0.07 - 0.10

V.

(grain boundary, grain size, precipitation, defect, dislocation -§•)

Q-factor# ^^§<>1 7}^}v\. ZL$\} ^ ^ ^ > Q-factor -

Q-factor

S U M M A R Y

I. Project Title

Materials Characterization by Resonant Ultrasonic Spectroscopy Method

II. Objectives and Importance of the Project

For the several decades, various nondestructive methods have been

applied to characterize microscopic variations in materials. However, it

is not successful to give a satisfactory result to monitor the nuclear

material degradation by neutron irradiation embrittlement. Therefore it

is necessary to develop a more sensitive nondestructive characterization

method. The resonant ultrasonic spectroscopy (RUS) can be a possible

candidate for this purpose. The objective of the project is to develop

the RUS technology to determine the dynamic elastic constants with an

accuracy less than 0.1^. In addition, RUS technology can determine the

high temperature elastic constant as well as Q-factor by an improvement

of the present RUS system. This technology can also be applied to

characterize the microstructural variations, such as material degradation

including neutron irradiation embrittlement.

III. Scope and Contents of the Projects

The dynamic elastic constants of weld heat affected zone(HAZ) of SA 508

Class 3 reactor pressure vessel(RPV) steel, which has various different

localized microstructures was investigated by RUS. A high temperature

device for the RUS measurement was designed and fabricated. The high

temperature elastic constants of the RPV steel was measured.

- IV -

IV. Results and Proposal for Application

Through the measurement of elastic constants from the various

localized microstructures we can confirmed that the RUS method is very

sensitive to the microstructure of the test materials. By comparing the

RMS error of the range of 0.07 - 0.10 % for this measurement to the

general limit of 0.2& for the effectiveness of the measurement, we can

confirm the measrements were highly reliable.

RUS can also be used to measure Q-factor (mechanical damping) which

related to the microstructural variations (grain boundary, grain size,

precipitation, defects, dislocations etc. ). In order to get an accurate

measurement of Q-factor, environmental pressure and contact pressure

between ultrasonic sensor and sample should be measured and controlled.

Thus the vacuum system for the environment and a load cell to control

contact pressure should be attached for accurate measurement of Q-factor.

The complete RUS system can be use to determine the anisotropic elastic

constant, temperature dependence and Q-factor. These capabilities will be

useful to monitor the degradation of nuclear materials, including neutron

irradiation embrittlenient. In addition, RUS technology can be applied to

various areas, such as the nondestructive identification of the fluid

inside a vessel, nondestructive quality test for precision components as

well as nondestructive materials characterization.

- v -

CONTENTS

Chapter 1 Introduction 1

Chapter 2 State-of-the-art 4

Section 1 State-of-the-art of similar research 4

1. Case of foreign countries 4

2. Case of domestic area 4

Section 2 Evaluation of the specific technologies 5

Section 3 Technical status of the Project 5

Chapter 3 Study results and discussion 7

Section 1 Theory of resonant ultrasound spectroscopy 7

1. Elastic constant of isotropic materials 7

2. Elastic constants of anisotropic materials 8

3. Calculation of resonance frequency 10

3.1 Minimization of the Lagrangian 12

3.2 Solution for rectangular parallelepiped shape 17

Section 2 Calculation of elastic constant 21

1. Levenberg-Marquardt algorithm 21

2. Consideration of Error bars and goodness-of-fit 25

Section 3 Measurement of ultrasonic resonance frequency 27

1. Ultrasonic transducer for resonant ultrasound

spectroscopy 27

2. Q-factor in the resonant ultrasound spectroscopy 28

Section 4 High temperature for resonant ultrasound spectroscopy— 31

Section 5 Experiment of resonant ultrasound spectroscopy 35

1. Determination of dynamic elastic constants of RPV steel

- vi

weld due to localized micro-structural variation 35

1.1. Introduction 35

1.2. Preparation of Specimen 36

1.3. Measurement of elastic constants by resonant

ultrasound spectroscopy 40

1. 4. Experimental results and discussion 42

1. 5 Conclusion 56

Chapter 4 Accomplishment and contribution of the study 58

Section 1 Accomplishment of the study 58

Section 2 Contribution to technology development 58

Chapter 5 Application of the results 59

^1 1 Necessity of additional study 59

^1 2 ^ Application to the other research 59

Chapter 6 References 60

Appendix

1. Detail drawings of high temperature resonantultrasound spectrospopy system 63

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,5*

l

$) 7}<£7m ^ % 4

1 ^ -S-4W -*HH W d£> W 41. ^ £ | ^ 4

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2 *g Afl - 7 ] # A > % ^ £ £ ^ r^ ^ ^ 5

7l#^ 1 1 5

^ ^ 2 f 7

7

}7fl^ 7

2. 6)uo^ :a*)l^ Q^n^r 8

3. ^ ^ r s ) - ^ T f l ^ 10

3.1. Lagrangian 3]4x£f 7l»g<ifl 5]*> •g-'g^nH5 ^ 12

3.2 ^^-^A(|ofl nfl?t i^afg- ig «H 17

2 ^ ^ ^ 4 - r 4^1 21

1. Levenberg-Marquardt iKnelil 21

2. Error bars ^ goodness-of-fitofl tfltl 3 - ^ 25

3 ^ i-g-aVg-'g ^ 4 ^ r ^ ^ 27

1. 3^-sF§-^^ ^-^# ^« %^> 27

2. J ^ s F g - ^ 1 ^ ^ ^ ^ 1 ^ ^ Q-factor 28

4 ^ Jl^r 5i^3i>^-tg«.^ A 1 ^ B | ^||3|- 31

5 ^ J i - i - s } ^ ^ ^ ^ 35

-^^f.^^1^ 4^ 35

1.1. * ^ 351 9 11 TEJ ^ . H l _ - - - Qfi1 , u. s^X xj. ^ C o | — OD

1.3. ^ ^ a } * ^ ^ * ^ ^ ^l t> f > A ^ l ^ r ^H§ 40

- viii -

1.

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m ^^ ^ fl^ H 581 ^ ^^fll ^ ^ B ^ ^-S ^ ^ £ 58

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^ 59

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2 ^ Bf <=*^-o\)$) -§--§- 59

60

63

- IX -

1 S- M

Resonant Ultrasound Spectroscopy) £

t:Hf-7) ^]^r canonical geometry^]

Lord Raleigh 7}

3. a l ^ . ^ ] 1970

3 j

1 5] *o}7] A}4^> 1980^^1] o)^:e>lt:}. 1987^

Los Alamos ^ - ^ ^ ^ ^ i ^ l Dr. Migliori^ °M7\]

o l S ^ PC - oflAl ^ - ^ ^ 3 ^ § <Sp§S} ^ oife hardware^

^ ^ ^ ^ ^ T W ^A l^ f e software^ n^W ^ ^ ^ ^ ^ ^ r ^ ^ (RUS

Resonant Ultrasound Spectroscopy) 2J-.2. ^ ^ ^ ^ l ^ . ^ 1990\lc}|

S E

- 1 -

O.I*

ufl -ofl ^fl*fe c^o>*> # M - $ (grain boundary,

defect, dislocation, precipitation ^-) afl

mechanical damping

pulse echo

mechanical

s.t:|-. al^oil S.-g-aVg-'g^^igoJI^^. ^.ig^a).^^ H>7}^- (FWHM, Full Width

Half Maximum)^ ^ ^ § * } ^ <^1S Q-factorS

Q-factor# ^ 1 ^

damping jL2f7> S ^ £ ] J I $X°^S. o|e|*> ^ ^ - 3.3l*llo> ^ c } . o]

# ^ Q-factorl

^^ ^ 1 # 7H1**H

Q-factor

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0 = C44£4 = C55£5 = C66£6

(7)

2c\2

' C12(8)

Poison's ratio u

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A ,—v (9)(cn/c12)

bulk modulus # A^Ot^A £}*M hydrostatic

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iggofl ^*f ujgfl^^d] Sfl(non-analytical

solution)^©] 7f-^^ e|| o?aflfe -

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tg

r ^ J. D. Maynard [2]

71 4 ^ 1 4 . Lamb ^ Love 6\) $\^ 7 ] ^ ©l^ofl o|oj 7]^ . »o>^Al«y A] ( 1 )

M #Sti^.^ Fraser and

[3]. ol*: Anderson, Kumazawa

rfl 1960

. Holland [4]^- Dermarest [5]fe <>1^ •%-*}?>± formalism#

^ # ^ r Ohno |

Mochizuki [7]7}

L^]#el ^-o>6fl^l n l ^ LOs Alamos

igliori^- Visscher7> <^5i 7fx| ^ S \ %$ cfl^Hl ^ ^ ? > ^

# ^-§-*H ^ m ^ ^ ^ * > 5 i 3 . <>1# i ^ s f g - i g ^ ^ ^ (RUS,

Resonant Ultrasoniat Spectroscopy) B}3. x^x^^}^-\ [8].

mechanical Lagrangian£) sfl

(eigenfrequency)-l-

11 -

3.1. Lagrangian £\£.Q

Lagrangian L •&

L= f(KE-PE)dV , (12)

cm

KE= \ ^po)2u) , (13)

y, z

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1st order

dx.

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(15)

(16)

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(17)

stationary point L

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bgr *J (17)51

6\

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Rayleigh-Ritz

(20)

Demarest [5] 3f Ohno [6]fe ^•fl-*!-^ Legendre

polynomial^ 4-§-*>^lfe 31 dl uov^^r ^ - # ^ ^ 1 matrix A^t ^]^>^1 ^ l^f l^ l

Sir}. Visscher et. al

(2D

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o] Lagrangian L

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Vibration Modes(Rectangular Parallelepiped)

k=l x-axis translationk=2 y-axis rotationk=3 z-axis rotationk=4 x-axis rotationk=5 volumetrick=6 z-axis translationk=7 y-axis translationk=8 complex motion

- 20 -

->

set

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steepest descents^] ^ Ho^-£.3. HJ3.2) -#-<*l^o] 9l°.v\

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- 26 -

mm l 4 \ & ] M ^ ^

g ^ > B ) ^ M ^ §]51 geometry

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S ^ 1 MHz

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Q-factor 7} ^^Sr | ^ ^ - ^ ^ 1 ' Slc>.

match7f -f^r^v) 7l7iH Q7f 50

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j>}$) x]^o]} greased - ^ * H

& Curie

- 27 -

(Lithium Niobatefe 800 - 1100 K <>M ^ 7 l ^ ^ S short $\S.7\ 5\7\\-\ -g--g-

Q) ^r£6fl 11> ^ 1 1 - *M*}7l ^ a o^-^5 - buffer rod

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rod :?H1 7^flxlfe ?Q$] o]v\. -7-^)1^ o^ z}o\ 20 cm, « | ^ 3 mm^ <g

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0.438 - 1.25 MHz o\]*\ T-M^c}. O\ ^ S } ^ ^^<Hl>H buffer rod

reverberation Iimit7> *Xt\. o\7%.~§: cfle>

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rodS # 41 Sllt:>. n}eM <^^-nlL| buffer rod#

M rod S] ^-^1 # ^ ^ - nle} ^ 4 *

^ s f | ^ ^ c K • a t ^ ^ S MHz

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2. J i ^ - s F g - ^ ^ ^ •^ 'H l^^ Q-factor

Q-factor

§ }. Q-factor fe ^-«g i ^ j

(FWHM; Full Width Half Maximum) J£fe ^/r •# ( / = ^ -^ ^rSHr, r =

- 28 -

J7Sfl

(thermodynamic dissipation)^- JS/ sfl

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Q-factor ^

(FWHM), ^ ^ ^ J # ^ ^ * f e 5 ^ £ ^ Q-factor

, ii) #Q2§ (grain boundary, inclusion, defect

., (elastic and non-dissipative) JS.71,

radiation,

- 29

mm 3.7}$]

radiation^

7}

Shear SJE.

T&$] 3.717}

$\ 3.7]±r gas

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^ radiation o|

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order ^cflA]^ ^ 51^}. 7 1 ^ 1 cfl^; Q

50K ol^} ^£6l|XI 7l<& (He

Q-factor ^ A^l &x\}7\ ^ c } . Isaak, Cynn, and Andeson [ 9 ] ^

^1 3*} fHJ 7^1^(third order elastic constant)# ^ •W&fe- tfl

bar *W ^ ^ 1 ^ 1 fe *^> Q ^ *i

- 30 -

l ^ ^ ^ r Fig. 4-1*11

synthesizer,

l^^ l B > Silfe § V § ! ^ g ^ | ( ] ^ Quatrosonic

Ruspec ^H])6fl 4 i ^ 7f<iS. ^ ^rJE 1<H ^ 1 # ¥ ^

Curie

-£-.§. wave guideS 4~§-*H 5.-B"47> furnace

^ ^ ] f e F i g .

wave guided] ^ ^ * H 4 ^ ^

31 W a M wave guide#

& holding ^ f e ^

fe 1000 °C 7}*1

- <% 500 °C ^ ^ 4 ^

31 ^ r ^ ^ ^ l 7fe*}J£-^ ^SftcK Fig. 4-3 £ 4-4 afl

Q ^ i

o}e\*} *}*£& ^^611 «><g*>7l ^ l ^ H 2*1- te^l^ife ^ ^ load cell-i

- 31 -

MicrcPro©

Prir

>essor

r

iter

p Synthesizer

DigitizerL

Receiver

Test 7Object VS.

Driver—, Transducer

spa Receive

Transducer

Fig. 4-1. Block diagram of resonant ultrasound spectroscopy (RUS).

32 -

ReceivingTransducer

Specimen

Wave Guide(Alumina Rod)

Thermocouple

TransmittingTransducer

Fig. 4-2. A design of high temperature device for RUS experiment.

- 33 -

Fig 4-3.

Fig. 4-4. furnace il wave guided SA 508

- 34 -

5 ^

1. #*}$.

1.1. *m

. alfe -#-§- 3»*>S ^^-§-71 (reactor pressure

vessel, RPV)fe ASME SA 508 Cl. 3 i&£#(Mn-Mo-Ni

(heat affected zone, HAZH tflsfl

[10.11].

[12].

1 6 l € - £ J. D. Maynard [13]

Holland [4]^- Demarest [5]fe ^ > ^ ^ ^ - S ^ » o ^ ^ l ^ ^

cfl ol ^ a j ^ g ; Ohno [6]ofl

Visscher

7>*1 Ji-i-31}- u o ^ 7> rc-il 3.^-2> ^ - ^ ^ (resonant ultrasound

- 35 -

spectroscopy ; RUS)-b

^ * 1 H * ! £ ?}¥*}** i < 8 ^ 371(1 mm

[14].

(anisotropic elastic constant)^ ^-^^fe ^ d ] 7 } ^ H [15,16]

3.7} 5

a]el

5J r>S.

1.2.

xf-g-51 ^ 1 ^ ^ ^ i ^S-8 - ASME SA 508 Cl. 3 ^ Mn-Mo-Ni Tfl

^: Table 5 - 1 ^ £v\ [17]. ^4^}S-§- ^ ^ ^ - ^ S^flfe i 6 j 5l

^•(quenching & tempering)<Hl ^*H S^Bfe tempered bainite

T:}. *>^ o]$\ - § - ^ ^ - ^ S^f|5l ^^7)1 220 mm!- <$ 130 pass

(post weld heat treatment)^ 7 l ^ ^ ^.d

(unit

- 36 -

SI Fig. 5-

Table 5-

mm X 3.5 mm X 4.0 mm

si 3.0

- 37 -

Table 5-1. Chemical composition of SA 508-3 steel

Elements

wt. %

C

0.19

Si

0.08

Mn

1.35

P

0.006

S

0.002

Ni

0.82

Cr

0.17

Mo

0.51

Table 5-2.

-*1 1 Identification

SI

S2

S3

S4

S5

S6

S7

S8

Thermal cycle simulation

(I*} 3l 2*} thermal cycle

1350° C

1350° C

1350° C

900° C

900° C

700° C

650° C

Base c

& 1350 ° C

& 950 ° C

& 750 ° C

& 900 ° C

& 700 ° C

& 700 ° C

& 680 ° C

naterial

CGTM

(TM)+TB

(TM) + TB

FGTB

FGTB + (TB

TB + (F) +

TB+CC

TB

+ F

* F)

CC

%CGTM: Coarse Grained Tempered Martensite

*TM: Tempered Martensite

*TB: Tempered bainite

*F: Ferrite

$FGTB: Fine Grained Tempered bainite

*CC: Coarse Carbide

- 38 -

S1(CGTM) S2 ((CGTM)+TB) S3 ((CGTM)+TB+F) S4(FGTB)

S5 (FGTB+CTB+F)) S6 (TB+(F)+CC) S7(TB+CC) S8CTB)

Fig. 5-1. Microstructures in various HAZ regions in SA 508 RPV weld.

- 39 -

1.3.

7M2

[14].

^ Levenberg-Marquardt»g#

merits a]

* H

Fig.5-2<H1

3 .3^ 'RPMODEL' 3:71

H7f degenrate

*1H4.5 mm

'RUSPEC'#

figure of

£.7]

Tfl

^ 3 . 5 mm X 4 . 0 mm X

2 " g 'RPR' JEEfe 'RPMODEL'

Levenberg-Marquardt^<^1

97fl<y orthorhombic symmetry

7 ^ * 1 SA 508 Cl. 2

- 40 -

Determine MaterialsStructure

(Isotropic, Cubic, Etc)

Prepare RectangularParallelepiped Sample

Determine Initial Estimateof Mode Resonant Frequencies

'btain Measured Frequencies

Run RPMODEL &Evaluate Error

\

Input Measured Frequenciesinto RPR using RPMODEL as

the Interface

Remeasure Missing or LargeError Mode Frequencies

\

/

Output Elastic Moduli

- Literature- lab Experience-Other Measurement

- Input Weight or Densityand Dimension to betterthan 0.1% Accuracy- Input Elastic Moduli "Guesses"Obtained from Literature orother Experiments

Iterate UntilError is

Acceptable

Fig. 5-2.

- 41 -

1) E - 207.200 - 57.09 T/1000 (GPa, T=° C /# ^ - § - « H [18], 25°

Young's modulus-H -r^}1?!,

E = 205. 77275 Gpa.

2) -&uo^ I ^ ^ I T 1 5i PQisson's ratio 2/ = 0.30 3. 7}^}3. 4 4 shear

modulus (7, Lame constant ^ , elastic stiffness eu , c12/ £44 -

= 75. 143 GPa,

*= MX. ,V1_O.A ~ 118- 7 1 5 °Pa>

1.4.

7.001 Gpa,

c12 = A = 118.715 GPa,

cu = -i- (c u - c12) - 79.143 GPa.

- 42 -

H (k)

5 -

4 -

2 -

1 -

0 -

500.0k 1.0M 1.5M

Frequency2.0M

Fig. 5-3. Typical resonance spectrum of SA 508 rectangular parallelepiped

shaped specimen.

- 43 -

SA 508 Cl. 3 #aovt8 *flfi°fi tfl*> ^ 4 * 1 ^ ^ 4 ^ - ^ ^ r ^ ^ S ) ^ ^ Fig

J ^ Table 5-3 <Ml ^ ^ 4 * 3 3 } } l

^ H r ^ o f l *NI3$i * § * A^KRMS e r r o r ) ^ ^ 4 i 0.07

0.14XS. ^-^SlSacK «aa>4AS. ^ 5 : ^.^}7> 0.2% fl

Fig. 5-4 91 Fig. 5-5<Hl Young's modulus ^ shear modulus

C>. 4 *]^ofl cflt!: Young's modulus $} shear modulus^ -H

JiSJ^K S?> Young's modulus^ ^.7] ^^§^2f -g^l ^ a H - H] Lsfl j £ £ 205

GPa ^ § £ S ^ ^ § € ^o l ^ ^ . a ^ i g ^ ^ i g ^ S ^ ^ « > ^-?-^lfe 209 ~ 212 GPa

71 >0

Fig. 5-4 5l Fig. 5-5<Hl-H 4 4 ^ o f l ^ ^ Young's modulus Q shear

modulus

J i 6 | a | o] ^ ^ - ^ % > ^ Young's modulus^)- shear modulus<Ml

fi^ 1350

l K ^ ^ 900°

2^}

S6-S7-S: 750

^7iuK5»), ^Bfl7f £]x l^ *tSJt^1^ tempering

(57)olc}. ^#^<?1 nl^l ^ 4 ^ ^ ^ # Table 5-2*11

5} ^t:]-. o]z\Q n}4] 3L^$] X}O]^. E > A ^ ^ ] ^ ^ <£3f*H A ^ tempered

martensite(57-S3) J£t:]-b tempered bainite(5^~55)^

tempered bainite ^ 4

S5, S6, S7

- 44 -

Table 5-3.

Speimen

No.

SA5O8_1A

SA5O8_1A1

SA5O8_1B

SA508 1B1SA508 1CSA508 1C1SA508 IDSA508 1D1SA508 2ASA508 2A1SA508 2BSA508 2B1SA508 2CSA5O8_2C1SA508_2DSA508 2D1SA508 3ASA508 3A1SA508 3BSA508 3C1SA508 3CSA508 3C1SA508 3DSA508 3D1SA508_4ASA508 4A1SA508_4BSA5O8_4B1SA508_4CSA508 4C1SA508_4DSA5O8_4D1SA508_5ASA5O8_5A1SA508 5BISA5O8_5B1SA508_5CSA508 5C1SA508_5D

[1012

dyn/cm2]

2.7661

c12 [ lO"

dyn/cm2]

1.1244

2.76461 1.125

2.7654

2.7611

1.1282

1.12392.7681 1.12872.7546J 1.11612.7554J 1.1182.75872.724

2.72262.7398

1.12171.09571.0931

1.112.7419J 1.11062.7528 1.12362.7678 1.13772.7732| 1.14722.7801 1.15342.7565 1.1265

2.757J 1.12672.76781 1.13832.7658! 1.13592.75511 1.12542.7567i 1.12592.758 1.1273

2.7619 1.13062.7534 1.12432.7566; 1.1263

2.757: 1.12922.7567 1.12822.7602 11.12752.7629 1.13242.7613 1.13242.7681 1.13842.7687: 1.12992.7653 1.12612.7676 1.1278

2.77 1.1292.7685 1.12942.7718 1.13082.7723 1.1324

ISA508 5D1 j 2.7668 1.127

c« [10"dyn/cm2]

0.8208

0.8198

0.8186

0.81860.81970.81920.81870.81850.81420.81480.81490.81560.81460.8151

0.8130.8134

0.8150.81520.8147

0.8150.81490.81540.81530.81570.81456.81520.81390.81420.81630.81530.81450.81490.81940.81960.81990.82050.81960.8205

0.820.8199

Young's

Modulus,

E (Gpa)

211.607

211.383

211.159

211.083211.425211.086211.001

211.02209.548209.641209.971210.147210.143210.506210.181210.379210.288210.337210.426210.451210.244210.371210.374210.522210.134210.329210.078210.133210.611

210.46210.273210.471211.376211.355211.456211.617211.412211.649211.559211.441

Shear

Mudulus

(Gpa)

82.08

81.98

81.86

81.8681.9781.9281.8781.8581.4281.4881.4981.5681.4681.5181.3

81.3481.5

81.5281.4781.5

81.4981.5481.5381.5781.4581.5281.3981.4281.6381.5381.4581.4981.9481.9681.9982.0581.9682.05

8281.99

BulkModulus,B (Gpa)

167.17

167.153

167.393

166.963167.517166.233166.38

166.737163.84163.62

165.327165.443166.667

168.1168.92

169.557166.983167.007168.153167.913166.857166.95

167.093167.43166.74

166.967167.18167.11167.18

167.582167.53

168.159167.617167.25167.44167.6

167. 57167. 78

167.897167.36

Poisson'sj RN6Ratio j error

<*)

0.28903J 0.106

0.28923J 0.0816

0.28976J 0.0909|0.28929J 0-0807

0.28965J 0.11880.28836J 0.08020.28864J 0.08460.28907| 0.08040.28684| 0.22790.28646| 0.19280.28833] 0.14780.28883J 0.14540.28986J 0.12140.291291 0.12640.29262[_0.13270.293211 0.12120.290111 0.10530.29009| 0.10160.29143| 0.1210.2911l| 0.1145

0.29| 0.08450.289991 6.08630.290161 0.11690.29044J 0.10610.289961 6.10710.29005! 0.11580.29057| 0.09860.29043 0.09640.29004J 0.11960.290691 0.07780.29081 j 0.10130.29139J 0.09890.289821 0.08090.289381 0.06890.289521 0.07050.28956! 0.06940.289731 0.07390.28976! 0.08280.289991 0.09330.289431 0.07

Density[g/cm3]

7.8838187.883818

7.837368

7.8373687.8497.849

7.8579267.8579267.8425497.8425497.8893137.88313

7.8502967.8502967.8221547.8221547.8384667.8384667.8346247.8346247.8460367.8460367.8483987.8483987.8387967.8387967.8219427.8219427.8656657.8656657.8443277.8443277.8369497.8369497.8694137.8694137.8527157.8527157.8481727.848172

Index

1

1

1

111112222222233333333444J

1 444445555555

5

- 45 -

Table 5-3. (?lHf).

Speimen

No.

en L10 |Ci2 LIU

dyn/cm ] dyn/cm ]

=„ [10"dyn/cm2]

Young's

Modulus,

E (Gpa)

Shear

Mudulus

(Gpa)

Bulk Poisson' RMS

Modulus, !s Ratio error

B (Gpa) I (%)

Density | Index I

[g/cm3] i

SA5O8 6A 2.76051 1.1221 0.8192 211.191 81.92J 166.8231 0.28901; 0.0642 7.83646JSA508 6A1 2.7636J 1.1237 0.82 211.404 82| 167.0271 0.28905: 0.0696 7.83646!SA508 6B 2.754J 1.1164 0.8188 210.996 81.88! 166.2271 0.28845; 0.0864 7.823086 6!SA508 6B1 2.7573! 1.1203 0.8185 210.996 81.85! 166.597| 0.28892; 0.0594 7.823046SA508_6C 2.75661 1.118 0.8193 211.141 81.93! 166.42] 0.28855; 0.0841 7.843055

81.98! 166.733] 0.28878i 0.10247.843327SA508 6D 2.7604! 1.1208 0.8198 211.308 6!SA508 6D1 2.764SA5O8 7A 2.7459SA508 7A1 2.7477!

SA508 7B 2.7571;SA5O8_7B1SA508 7C

2.7608

1.1252 0.8194 211.293 81.941 167.147| 0.28931 j 0.0696 7.8433271.1116 0.8172 210.535 81.72! 165.63J 0.28815; 0.0795 71.1125 0.8176 210.646 81.76i 165.757 0.28882! 0.075471.1212 0.8179 210.873 81.79; 166.657

2.7462!1J2571.1096

JUS1750.8183

210.86210.757

81^75!81.83!"

167.080.289111 0.11437

165.513|0.28966J

~o] 28777!0.088170."'1024 7,

,817048.817048!"817048f8170481823595F

_77

it7!

SA508 7C1 2.7506 1.1148 0.8179 210.757 81.79J 166.0071 0.28841 0.07487.823595]U

SA508_7D 2.7519 1.1148 0.8186 210.919 81.86| 166.043! 0.28829;SA5O8_7D1ISA508 8A

2/7551J2.74681

0.8182 210.897 81.82; 166.417!1.1121 0.8174 210.59 81.74J

81.79"165.93j

0.28879;0.28817!

7.818946[ 707967.818946! 7

0.10410.0.0743 7.829797!

SA508 8A1 2.7479! 1.112 0.8179 210.709 165.737! 0.28811; 0.0739 7.829797!;SA5O8_6C1SA508 8B

2.7563! 1.1181 0.81912.7612; 1.1268 0.8172

211.096210.807

81.9181.72

166.4171167.16!

0.2885910J28981!

0^057370.0805 7

843055!8178351

SA508 8B1 2.762! 0.818 210.98 81.8 167.133! 0.28961! 0.08 7.817835!SA508_8CSA5O8_8C1SA508_8D "SA508 8D1

2. 7553; 0.8181 210.881 81.81 166.45! 0.28884; 0.0844 7.822957!2. 7537;2.750H

1.11691.116

0.8184 210.911 81.84U

0.8171 210.59 81.71166.25! 0.28856! 0.0753 7.822957;166. 711 0.28864r~0.0753I7.813875!

2.7527! 1.1167 0.818 210.815 81.8 0.2886 0.0834 7.813875! 8!

- 46 -

212.0i

O)

0 1 2 3 4 5 6 7 8 9

Specimen Group

Fig. 5-4. Young's modulus of SA 508 Cl. 3 alloy by WS.D

! I! I

i !

0 1 2 3 4 5 6 7 8 9

Specimen Groups

Fig. 5-5. Shear modulus of SA 508 Cl. 3 alloy by RUS.

5 i: 1350C-1350C,S Z 1350C-900C,S Z 1350C-750C,S £ 900C-900C,S S 900C-750C,S 6:750C 750C,S T. 680C-680C,S X raw material

47 -

tempered martensite(Si ~S3)$) t M ^ ^ f e ^ ^ -3.7H cflfjflA-J <*>;?>

7fl^r7} pearlite-bainite-martensite£) ^A-j.3. 4 4 : * H tempered

martens i t e ^ H f e v}X\ ^7>*>t|- pearliteS}

2 ^ [19] <£xmr.\.

Fig. 5-6 51 Fig- 5-7<Hl 4 4 ^1^*1) ^«>

^ 7 | « t > « ^ I ^ S . C^- A)^#2ffe ^51 SI*]} tbQ cUr

scattering*}3. Sl-c- 1 d]*fl tfltl ^ ^ 1 ^ : ^ r^^l ?it:>. J£SV Young's modulus

7} specimen group<Hl v%$ ^ ^ « > * H t ^ - ° f e ^ ^ °H1 ^ S " * f e cu^r C>

^}^^} . °lfe stiffness ^ ^ , cs <$W off-diagonal ty<& c122] «g

Young's modulus, E-b c,y5| ^*J^^1 S« # ^ S l ¥) £ = 1 / S U

&<$ da # 0 61 ^ . f Cll2f^ c}^ . ^o ] Tfl^ig ^ jJlcK C44

shear modulus(Fig. 5-5)^-

Sife tfl Fig. 5-8 gj Fig. 5-9<Hl 4 4

Tfl s ca t t e r ing*^ $1^ cfl < lfe

^ 44

* f e cfl dl<>1lfe 1) martensite^l tetragonality£] 4 ^ 5J ^ T S , 2) #$1 4

4i, 3) carbide <Qx}*\ "&% ^ 7-AoV f ^ & ^ ^ « ^r Slc}[20].

martensite S ^ J i c f e bainite 2I^°L3. %^r^, £3!^SJ 3.7]7\ 4

S73} •%•*}# tempered bainite

307fl

- 48 -

2.78-

2.77-

V" 2.76-

jo" 2.75-O

S, 2.74-

° 2.73-

2.72-

2.71-

•

•

•

:

s

J•1

•I

i ,i<

ii •

; :

tt

at••

••

1 2 3 4 5 6

Specimen Group

Fig. 5-6. Elastic stiffness ( cn) of SA508 Cl. 3 alloy by

1.16-j

1.15-

1.14-

"t 1.13-o

I 1.12-j

>< 1-11-

o" 1.10-

1.09-

1.082 3 4 5

Specimen Group

Fig. 5-7. Elastic stiffness ( C-Q) of SA508 Cl. 3 alloy by RUS.

S l: 1350C-1350C,S 2: 1350C-900C,S 3: 1350C-750C,S 4: 900C-900C,S 5: 900C-750C,S 6: 750C 750C,S 7: 680C-680C,S 8: raw material

- 49 -

5970

5960-

!F 5950-

— 5940-

'o•§ 5930-

o>5 5920-

73

O) 5900-o

5890

: !

3 4 5 6

Specimen Group

Fig. 5-8. Longitudinal wave velocity of SA 508 Cl. 3 alloy by RUS. 3)

I1IS

3235-

3230-

3225-

3220-

3215-

3210-

•

••

•

•

!

s•t•••

••••

1 1

1•1

• •

• ••

•

3 4 5 6

Specimen Group

Fig. 5-9. Shear wave velocity of SA 508 Cl. 3 alloy by RUS.

S i: 1350C-1350C,S Z 1350C-9WC,S X 1350C-750C,S 4: 900C-900C,S S 900C-750C,S K 750C 750C,S 7. 680C-680C,S & raw material

- 50 -

v}*\] ^2:5} lattice distortion, ^ ^ ^ 37] ^

K Palanichamy et al.^r [21, 22] i ^ M ^ B

lattice distortion, ^ ^ ^ , *1# - <>1 db*f7j nfi^-0!^^! JL2.*}9Ji:f. Ahn

and et al.^r [23] t>*fi ^^>^ 7O H1^ ^ ^ 4 ^ £ 5 } ^ ^ ^ j 3.7],

} martensite ll<Hl ^ S ^ U ^ 3 .71^ - - Bfl < 1 <H1 ^cfl»> austenite

37)$} 2*^*1 # ^ Sife cfl ^ 1 3 . bainiteU martensite

fe ferrite+pearlite

ferrite+pearlite+bainite S ^ , bainite+martensite

[24] <HH-£ retained austenite + martensite

3 . martensite ^ , martensite + bainite -#,

ferrite + pearlite + bainite ^h ferrite + pearlite

Fig. 5-10 ?1 5-llofl ^ r £ ^5f<Hl 4^r Young's modulus «! shear modulus^]

l A ^ Fig. 5-12 iJ 5-136fl £5. ^Sf6fl tc>s. ^ , 4 ^ £ ^ ^ 1

-S.O}- Young's modulusif shear modulus^

nfl -ofl ^}5|*1 ^4>o) ^>EJ) Al^oj) 5 | ^ ^%>?]x] ^ ^ * > data scattering

Fig. 5-lOofl-M 7 l ? H A|^6]l S]*> Young's modulus^ £5. S]^ Tfl^ £• 207.200 - 57.09 T/1000 (GPa, T=° C)

- 51 -

^ l ^ ^ -57.09 MPa/°

^ -70.27 MPa/° CS.

- 52 -

215-,

210-

185-

SA5081BSA508 1A

s.to33

lod

(0"CDc

1

205-

200-

195-

190-

E=207.2-0.05709T

. E=214.54-0.07087T

0 50 100 150 200 250 300 350 400 450

Temperature [C]

Fig 5-10. Variation of Youngs modulus of SA508 Cl. 3 steel.

[GP

a]M

odul

usS

hear

8 2 -

8 0 -

7 8 -

7 6 -

7 4 -

7 2 -

7 0 -

t

•

t

SA508 1BSA508 1A

•

• #

50 100 150 200 250 300 350 400 450

Temperature [C]

Fig 5-11. Variation of shear modulus of SA508 Cl. 3 steel.

- 53 -

5950-

5900-

5850-

5800-

t

2 5750-

5700-

5650

• SA5081B• SA5081A

50 100 150 200 250 300 350 400 450

Temperature [C]

Fig 5-12. Variation of longitudinal wave velocity of SA508 Cl. 3 steel.

3250-,

3200-

3150-

"o

I0) 31C

Ira^ 3050-

co

3000-

SA5081BSA5081A

0 50 100 150 200 250 300 350 400 450

Temperature [C]

Fig 5-13. Variation of shear wave velocity of SA508 Cl. 3 steel.

- 54 -

Zirconium ^ # 2 } ?l7ll^4; 3.-g-£(Terminal Solid Solubility: TSS)

1.5. £^

M *> ^ ] B I SA 508 Cl. 3

4 ^r*

*>Sgl .t -^^ -i-^ Young's modulus 209 -212 GPa^ ^^m^l 3L7]

205 GPa 1 4 ^>^V ^5tt4.

— ^ tempered martensite S^jjtcl- tempered bainite

3. ^i-sVg-ig& S L ^ % 4 ^ S f e ^ ^ ^ ' ^ 3717} # i * K ^ , martensite

bainite 2 2 , ' ^ ^ ^ ^ - ^-^<>1 ^7>*

4. Young's modulus gj shear modulus^-

5.

- 55 -

Zirconium ^^$] rS.<H] ty^ Sb!|*f4i 5L%&.(Terminal

Solid Solubility: TSS)£| ^ifi ^ - ^ # t\<gQ ^-§-o] 7 > ^ * H ^*1 7]^]X\

- 56 -

7ii

. o]

- 57 -

mechanical Q-factor7} iLt:>

«fl ti4tt ^ ^ ^ Q-factor#

Q-factor

wave guide

71

1) Load cell#

2) 1^- l^^l

Ef o Qo o

. -§-71 71

- 58 -

1. L. D. Landau and E. M. Lifshitz, Theory of Elasticity, 3rd ed.

(Pergamon Press, London, 1986).

2. J. D. Maynard, "Resonant ultrasound spectroscopy", Phys. Today, 49, pp.

26-31 (1996).

3. D. B. Frazer and R. C. LeCrew,"Novel method of measuring elastic and

anelastic properties of solids",Rev. Sci. Instrum., 35 (9) pp.1113-1115

(1964).

4. R. Holland,"Resonant properties of piezoelectric ceramic rectangular

parallelepipeds", J. Acoust. Soc. Am., 43 (5) pp. 988-997 (1968).

5. H. H. Demarest,"Cube-resonance method to determine the elastic

constants of solids", J. Acoust. Soc. Am., 49 (3) Pt. 2, pp. 768-775

(1971).

6. I. Ohno,"Free vibration of a rectangular parallelepiped crystal and its

application to determination of elastic constants of orthorhombic

crystals", J. Phys. Earth, 24, pp. 355-379 (1976).

7. E. Mochizuki,"Sphere-resonance method to determine elastic constants

of crystal", J. Appl. Phys. 63 (12) pp.5668-5673 (1988).

8. W. W. Visscher, A. Migliori, T. M. Bell, R. A. Reinert, "On the normal

modes of free vibration of inhomogeneous and anisotropic elastic

objects", J. Acoust. Soc. Am., 90 (4) Pt. 1, pp. 2154-2162 (1991).

9. D. G. Isaak, 0. L. Anderson, J. D. Carnes, and H. Cynn, "Elasticity of

fused silica shperes under pressure using resonant ultrasound

spectroscopy", J. Acoust. Soc. Am. 104 (4) pp2200-2206 (1998).

IRHAZ £| n | 4

37 (8) pp. 1000-1007 (1999).

11. 3 ^ , ^ « h " S A 508 Cl. 3*}s§3} n]M] 3 ] ^Sf", cfl^^^-^SIxl, 36 (8) pp. 1329-1337 (1998).

12. A. Miglioli, W. M. Visscher, S. E. Brown, Z. Fisk, S. -W. Cheong, B.

- 59 -

Alten, E. T. Ahrens, K. A. Kubat-Martin, "Elastic constants and

specific-heat measurements on single crystals of La2CuO4", Phys. Rev. B,

41 (4) pp. 2098-2102 (1990).

13. J. D. Maynard, "The use of piezoelectric film and ultrasonic resonance

to determine the complete elastic tensor in one measurement", J. Acoust.

Soc. Am., 91 (3) pp. 1754-1762 (1992).

14. A. Miglioro, J. Sarrao,"Resonant ultrasound spectroscopy", John Wiley

& Sons Inc. (1997).

15. Y. -M. Cheong, S. -C. Kwon, H. -K. Jung,"Determination of anisotropic

elastic moduli of Zr-2.5Nb CANDU pressure tube materials", J. Mater.

Sci., 35 (5) pp. 1195-1200 (2000).

16. ;§-§-?-, 1 , £<3*J, ^ W , " ^ * } ^ ^ ^ o]-§- Zr-2.5Nb ^

pp.13-27 (1999).

17. ASME B & PV Code Sec. II, Part A, SA 508 (1995).

18. D. R. Ireland, W. L. Server, R. A. Wullaert, ETI Technical Report No.

75-43, pp.5-10 (1975).

19. E. P. Papadakis,"Ultrasonic attenuation and velocity in three

transformation products in steel", J. Appl. Phys., 35 (5) pp.1474-1482

(1964).

20. R. Prasad, S. Kumar,"An investigation into the ultrasonic behavior of

cast and heat-treated structures in steel", British J. NDT, 33 (10)

PP. 506-509 (1991).

21. P. Palanicharmy, M. Vasudevan, T. Jayakumar, S. Venugopal, B.

Raj,"Ultrasonic velocity measurements for characterizing the annealing

behavior of cold worked austenitic stainless steel", NDT&E Int., 33, pp.

253-259 (2000).

22. P. Palanichamy, A. Joseph, T. Jayakumar, B. Raj, "Ultrasonic velocity

measurements for estimation of grain size in austenitic stainless

steel", NDT&E Int., 28 (3) pp.179-185 (1995).

23. B. -Y. Ahn, S. S. Lee, S. T. Hong, H. C. Kim, S. -J. L.

Kang,"Application of the acoustic resonance method to evaluate the grain

- 60 -

size of low carbon steel", NDT&E Int., 32, pp. 85-89 (1999)

24. *]&q, *}&<$. ^ , tf<3«. ^^<i,. pp. 27 (1995).

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BIBLIOGRAPHIC INFORMATION SHEET

Performing Org.

Report No.

Sponsoring Org.

Report No.Stamdard Report No. ! INIS Subject Code

KAERI/RR-2077/20001l

Title / SubtitleMaterials Characterization by Resonant Ultrasound

Spectroscopy Method

Yong-Moo Cheong(NucIear Materials Technology)Project Manager

and DepartmentResearcher and JH.K. Jung(Quantum Optics Lab.), Y.S. Joo(KALIMER), C. M.

Department ]Sim(HANARO),

Publication

Place

Page

Taejon i Publisher KAERIPublication

p. 72 !! 111. & Tab. | Yes( o), No ( )

! Date

I Size

2001

Cm.

Note

Classified Open( o ), Restricted( ),

Class DocumentReport Type Research Report

Sponsoring Org. Contract No.Abstract (15-20;

Lines) j

A high temperature resonant ultrasound spectroscopy(RUS) was developed. The dynamic

elastic constant of RPV weld, which has various different microstructure was determined by

RUS. It was confirmed the RUS method is very sensitive to the microstractures of the

material. RUS can be used to monitor the degradation of nuclear materials including neutron

irradiation embrittlement through the measurement of dynamic elastic constants, elastic

anisotropy, high temperature elastic constant and Q-factor.

Subject Keywords

(About 10 words)

Resonant Ultrasound Spectroscopy, Elastic Constant, Material

Characterization, Nuclear Materials