40

(Stress Corrosion Cracking,

SCC)(Vessel
Internal CrackingVIC) VIC

(Fatigue)(Wear)
(1)(2)

IGSCC IASCC

SCC

(Hydrogen Water
Chemistry, HWC)(3,4)HWC
( 0.6ppm )
-16
-60

HWC

IGSCC HWC
(5-13)
(Primary Coolant Circuits, PCCs) HWC

(Catalytic)(Inhibitive)(5,11,12)
IGSCC

(Noble Metal Chemical,

NMCA)(19-23) Pt

NMCA

NMCA

(7,8) IGSCC
HWC

 HWC
IGSCC
(ZrO2)(TiO 2)(ZrO(NO 3)2)
BWR
150 304
304
HWC BWR
304

2.1
BWR SCC

(Tensile Stress)(Corrosive
Environment)(Susceptible Material) 2-1
SCC
SCC

Tensile

Susceptible

stress

material
SCC

Corrosive
environment

2-1

2.1.1
BWR SCC
(1)
BWR
5


SCC
SCC
(HeatAffected Zone,HAZ)
SCC

(2)
BWR (Radiolysis)

SCC

(3)
BWR 304304L316316L
Inconel 600X-750
500 850

(Sensitization)

 HAZ

IGSCC

(Radiation-Induced Segregation, RIS)

IASCC

2.1.2
SCC
SCC
SCC

(1)

(2)

IGSCC
7

 BWR
0.1S/cm

IGSCC IGSCC
HWC

(3)
SCC
(<0.03%)() 304L
316L Nd Ta Ti (Strong
Carbide-Former) 347321

HWC
ZrO 2

2.2

M M n + + ne -

(1)

H 2 H + + e

(2)

O 2 + 2H 2 O + 4e 4OH

(3)

H 2 O 2 + 2H + + 2e 2H 2 O

(4)

(Radiolysis)

1
H 2O2 O2 + H 2O
2

(5)

(1)(3)(4)

ECP ECP
(3)(4)(1)

ECP Macdonald (Mixed

Potential Model, MPM) (25)MPM
9

iR /O , j ( E) + icorr ( E) = 0

(6)

j =1

iR/O, j j R/O icorr

/

R O + ne

(7)

R O
Butler-Volmer

iR / O =

1
i0 ,R / O

e ( E ER / O ) / ba e ( E E R / O ) / bc
1 ( E E Re / O ) / ba
1 ( E ERe / O ) / bc
+
e

e
i , f
i , r

(8)

i0,R/O ( ECD)i,f i,r

(Limiting Current Density)ba bc
Tafel E Re /O Nernst

10

i0, R / O = nFk0CO C R

(9)

F Faraday k0 (Intrinsic
Electrochemical Rate Constant)CO CR
(Transfer Coefficient)Tafel

ba = 2 .303 RT /(1 ) nF

(10)

bc = 2.303 RT / nF

(11)

R T (Turbulent Flow)

il ,O / R = 0.0165nFDCO / R Re0.86 Sc0.33 / d

(12)

()()D
(Diffusion Coefficient)CO / R O R (Bulk)
Re Reynolds (Reud/v)Sc Schmidt (Scv/D)d
u v

11

E Oe / R = E O0 / R

a
2.303 RT
log( R )
nF
aO

(13)

aR aO R O E R0 /O

ECP
( E Re /O ) Tafel (ba bc)
(i,f i,r)
(8) k0
(i0,R/O )

ECP
( i0, R / O )
i0, R / O = FI , R / O i0, R / O

(14)

FI,R/O ECD

2-2 ( Evans Diagram)

ECP
2-1 ABC A
B C
12

( A)( O1)
Ecorr1A ECP icorr1A (
)

BWR HWC

( B) O1
ECP(Ecorr1B) ECP
(icorr1B) ECP

ECD
ECD 3
ECD i0,1 H /H i0,2 H /H O1 3
+

O2ECD i0,1 O /O i0,2O /O

2

Tafel
()
A O2 ( ECP) Ecorr2A

13

 icorr2C
ECP

HWC
C O2 ( ECP) Ecorr2C
A icorr2C
ECP

ECD ECP

ECD

14

i0,2 O /O2
2

EO

2 /O

i01,O

A. Metal Oxidation
2
2 /O

C.

Metal + H2 Oxidation
Inhibitive Coating
B.

Ecorr1A
Ecorr2A

Metal +H2
Oxidation on Metal

Ecorr1B
O1

Ecorr2C
EH /H+

O2

i0,2H /H+

1
+
0,H2 /H

i0, M/M n+

EM/M n+

-12 -11 -10 -9

-8

-7

icorr2C

icorr1B

icorr2A

icorr1A

-6

-5

-4

-3

-2

-1

log i (A/cm 2 )

2-2 ECP

15

3.1
BWR

IGSCC BWR
200 300ppb
IGSCC
(26) BWR

ECP (27)ECP IGSCC

ECP (28)
-230 mVSHE 304 IGSCC (Ecrit )
ECP Ecrit

16

 HWC
HWC BWR
HWC

HWC ppb

ECP HWC
(Upper Downcomer)(10)

(28)-16
-60

BWR N16
HWC N16
NH3 NOX

17

 R. L. Cowan(24) HWC 304

..
MCr2O4 CoCr2O4
3-1 Co60
NWC
HWC Co60 3-1
3-1 (24)

3-1 NWC HWC Co60 (24)

18

3.2
200 300
ppb

3.2.1 (Sol-gel Method)

TiO 2(29,30) ZrO2(9,32,33)
TiO 2-SiO 2(34-37)
(38-41)(
)()()
Sol-gel
FormulaZr(OC3H7)4+C3H7OHCH3COOH
H2O
Concentration0.025 to 0.9M ZrO 2
Volume ratio H2O/ CH3COOH2

19

H2O/ C3H7OH1
Sol-gel 20

40 oC 70 oC 15
400 oC 1
Tg()
(Densification)

(Amorphous)(Porous) Sol-gel
(42-46) 1. (Spin Coating) 2. (Dip
Coating)3.(Spray Coating)4.(Electrophoresis)

2 Cr2O3

800 oC
Fe2O3
(38)

20

 X (X-ray Diffraction, XRD)

(Fourier Transform Infrared Spectrum, FTIR)
3-2(38) ZrO2
XRD (a)
(b)(c)T(111)
ZrO2 (d)
XRD
ZrO2 316L
40 nm

ZrO2 (38) Zr-O-Fe

ZrO2
3-3(38) 3-4(38)
ZrO2 FTIR (a)
(b)(c)
FTIR

Zr-O-C Zr-O-Zr
ZrO 2

21

Sol-gel TiO 2-SiO 2 (38) 3-5

(9) Sol-gel 304

(288 oC 0.1 S/cm )
ECP

3-2 ZrO2 XRD (38)

22

 3-3

(38)

3-4 ZrO 2 FTIR (38)

23

 3-5 1 mVs-115% 250C(a) 316L

SS(b)316L SS 8000C 2 (c) TiO 2 -SiO 2
316L SS (34)

3.2.2 (Plasma Spray)

(8,51) 200 ppb

(500 mVSHE) 200-300 ppb

3-6

(TiO 2) n-type
24

(410 nm) ECP

3-7(53) TiO 2

Evan Diagram 3-8(53) 3-9(53)

TiO 2 304
TiO 2
ECP TiO 2
ECP

(42) pin-hole
(microcrack)

(42)

25

 3-6 YSZ(Yttria stabilized zirconia)

ECP (8)

3-7 TiO 2 (410 nm)

ECP (53)

26

 3-8 TiO 2 ECP

Evan Diagram (53)

3-9 TiO 2
(53)

27

3.2.3. (Alloying)
(Zirconium) 304
0.5~3.0 wt
ECP (8)
ECP 3-10(8)

3-10 Zr 304
ECP (8)

3.2.4. (Chemical addition)

Kim 1 mM ZrO(NO 3)2 10 ppm

(8)

28

(288 oC 200 ppb2 )

60 oC 10 ppm 10
20 ECP 3-113-12(8)
ECP
100 ppb ECP IGSCC
(-230 mVSHE) 3-13(8) 1 mM ZrO(NO 3)2
(Auger Depth Profile) Zr

3-11 1 mM ZrO(NO 3)2

ECP (8)

29

 3-12 10 ppm
ECP (8)

3-13 1 mM ZrO(NO 3)2

(8)

(47)
()
pH 2.8 7.1 160 oC 6
12 (Interfacial Resistance)

30

 300 ECP
ECP 400 mV 3-14
B. Stellwag(48)
ZrO 2
ECP
K3Fe(CN)6/K4Fe(CN)6 ZrO2

3-15 ZrO 2

ECP
Kim ECP
Prefilm ECP 3-113-12
B. Stellwag ECP
3-16 ZrO 2
Prefilm ECP (54)
ECP Prefilm

31

 3-14 304 ECP

(47)

3-15 ZrO2
(48)

32

 3-16 ZrO2 ECP (48)

3.2.5.(Electrophoretic Deposition)
ZrO2 HCl
pH

ZrO2 (50) 150m

(Electrochemical Impedance Spectroscopy, EIS)
ZrO2
1000 3-17(Constant Load)
220 S/cm
ZrO2 400
3.9210-7cm/s ZrO2

33

 3-18 ZrO(NO 3)2

(52)

3-17 ZrO 2
()()(50)

34

 3-18 ZrO2
(50)

(11)

(12)

ECP

35

3.3 (SSRT)
SSRT
SCC
SSRT
ECP -
10-2sec -1SSRT 10-5~10-7sec -1
SCC

SCC

EPR EIGSCC
ECP EPR SSRT (31)
IGSCC ECP (EIGSCC) 3-19(31)
SSRT (18) IGSCC
(Crack Growth Rate, CGR) TGSCC

36

 3-19 EPR IGSCC EIGSCC

(31)

(13-17)
(Crack tip)
(Crack mount)PH
D. D. Macdonald (17)
(Induction stage)
(Crack propagation stage)

3-20

37

 3-21

3-20 (17)

3-21 (17)

38

4.1
304
304

4-1
650 24 SiC
1200

(Electrochemical Potentiokinetic Reactivation, EPR)

(24)(Degree of Sensitization, DOS)

4.2 (Insulated Protective Coatings)

288 300ppb
(prefilm)
10
10
39

Type 304 SS

650 24hr
+

14days 288 [O2 ]dis =300ppb

14 days 150

ECP

SSRT

[O2 ]dis=100~1000ppb

1.[O2 ]dis=300ppb,[H2 ]dis =10ppb

1.[H2 ]dis=0ppb, 2.[H2 ]dis =10ppb

2.[O2 ]dis=300ppb,[H2 ]dis =25ppb

3.[H2 ]dis =25ppb,4.[H2 ]dis =50ppb

SEM fracture surface examination

IGSCC% Max.stress Elongation
ECP value
AES maps, depth profile

4.1

40


150
ZrO2TiO 2 ZrO(NO3)2 10 ppm10 ppm
1 mM 14

4.3 (Recirculation Loop)

BWR

(SSRT)
SSRT (ECP)
ECP

4-2 SSRT
4-3 ECP

4.3.1
SSRT
316

41

 4000psi 15

(Damper)(Safety Valve)
(Heat
Exchanger)(Pressure Regulator)

ECP
ECP SSRT
ECP

4.3.2
SSRT

PULSAR
25HJ 2095psi
1.93 gallon/hour
42

Deionizer
Gas Vent

PC

Flower
Meter

IBM Compatible

Water

Keyboard

Tank

Multimeter
SSRT Contrller
Load

Conductivity

H2

O2

Cooler

Recirculation
Pump

Damper
Temperture
Controller

N2

H2 O 2

High
Pressure
Pump

Heat
Exchanger

4-2 SSRT
Deionizer
Gas Vent

PC

Flower
Meter

IBM Compatible

Mass Flow
Controller

Water

Keyboard

Tank

Switch System
Nanovolt Tmeter
Conductivity

H2

O2

Cooler

Damper

Autoclave

Recirculation
Pump
High
Pressure
Pump

Heat
Exchanger

Temperture
Controller

4-3 ECP

43

N2

H2 O 2

 1200psi
1500psi

1800psi

ECP
PULSA Series 680 1800psi
1 gallon/hour

4.3.3
1
1/4 1/2

500W220V 288
380
450 SSRT

ECP

44

4.3.4
SSRT

GLI Model C53

GLI Model C53

ORION Series1816 Orbisphere
Laboratories3600

ECP
GLI Model D63 SSRT

4.3.5

16M
BARNSTEAD D8901 High

45

Capacity Cartridge D8911 Ultrapure Cartidge

0.1S/cm

4.3.6
SSRT

SSRT

Parker

ECP

ECP MKS Model 247C 4-Channel MKS

Mass-Flow Controller

4.3.7
46

SSRT
KEITHLEY 2700 Multimeter
20 GPIP

ECP
KEITHLEY 2182 (NANOVOL TMETER) 7001
(SWITCH SYSTEM)
ECP

4.4
SSRT 4-4 316

1.6710-7 s -1 288 1100psi

40ml/min Linear Voltage Displacement
Transducer(LVDT) 20

(Scanning Electron Microscope,

HITACHI S-4000) IGSCC
47


304

4-4

4.5
ECP
316
1100psi 20ml/min
Conax
/
288 123 mVSHE
ECP
10

48

4.6
X (Energy
Dispersive X-Ray Spectrometer, EDX)(55) Auger
(Physical Electronics, Auger 670 PHI Xi)
IGSCC

49

304 5-1
650 24
5-2
DL-EPR (54) 24 650
46%
(prefilm) 150
10ppm ZrO210ppm TiO 2
1 mM ZrO(NO 3)2

5.1
(SSRT)
300ppb 10ppb
1 300ppb 25ppb
1 2 5-3
(ZrO2,TiO 2,ZrO(NO 3)2) SSRT

50

 5-1 304

Mass%

Fe

Cr

Ni

Mn

Co

Si

Cu

Mo

68.9

0.075

17.1

7.55

1.10

0.088

0.427

0.239

0.222

0.191

0.019

5-2 DL-EPR (54)

Sensitization Time
(at 650)

As Received

With Solution Annealing

(1050,0.5hr)

0 hr

2.67*10-2%

22%

6.1%

21%

5.3%

42%

8.8%

1 hr

8 hrs
35%
24 hrs

46%

5-3 SSRT

[O2]dis =300ppb
[H2]dis =10ppb

[O2]dis =300ppb
[H2]dis =25ppb

Prefilm

~ 0.5

>1

IPC-ZrO2

~ 0.5

>1

IPC-ZrO(NO 3)2

~ 0.5

>1

IPC-TiO 2

~ 0.5

>1

5.1.1

51

 5-4(54) 300ppb SSRT

90150200 5-1
150 5-4

IGSCC prefilm
IGSCC

5.1.2 300ppb 10ppb SSRT

5-5 300ppb 10ppb(
1) SSRT 5-2 300ppb
10ppb SSRT
Prefilm
Prefilm 280
155 MPa 9.65%
315~335 165~180 MPa
10.91%~11.55%
IGSCC Prefilm
IGSCC
300ppb SSRT IGSCC

52

 IGSCC
5.1.3 300ppb 25ppb SSRT
5-6 300ppb 25ppb(
1 2) SSRT 5-3 300ppb
25ppb SSRT SSRT

1 SSRT Prefilm
Prefilm 320
175 MPa 11.15%
339~345 180~186 MPa
11.77%~11.92% IGSCC
Prefilm IGSCC

1 SSRT
IGSCC
IGSCC
IGSCC IGSCC

53

 300ppb SSRT (54)

5-4

Time to fracture
(hr)

Elongation
(%)

IGSCC
(%)

Prefilm

220

7.55

52

ZrO2-150

320

10.97

40

295

10.11

48

308

10.56

42

ZrO(NO 3)2-150

TiO 2-150

400

100

350
ZrO2

ZrO(NO 3)2

Type304SS
[O2]dis:300ppb

TiO2

300

80

-7

288 C Strain rate=1.67*10 S

IPC

250

-1

60

Prefilm
ZrO(NO3)2

200
ZrO2

150

hr

Prefilm
TiO2

40

100
20
50

Prefilm

ZrO2 ZrO(NO ) TiO2

3 2

Fracture Time

Elongation(%)

IGSCC%

5-1 300ppb SSRT

54

 5-5

300ppb 10ppb SSRT

Time to
fracture(hr)

Max.
Stress(MPa)

Elongatio
n
(%)

IGSCC
(%)

Prefilm

280

155

9.65

40

ZrO2-150

335

180

11.55

32

315

165

10.91

30

322

172

11.11

34

ZrO(NO 3)2-150

TiO 2-150

55

400

100
ZrO 2

350
300

TiO
ZrO(NO 3)2 2

Type304SS
[O2]dis:300ppb
[H2]dis :10ppb

Prefilm

80

ZrO2
TiO
ZrO(NO3)2 2

200

-1

TiO2
ZrO(NO 3)2
ZrO2

Prefilm

Prefilm

150

60

hr, MPa

-7

288 C Strain rate=1.67*10 S

IPC

250

40

100
50
0

20

ZrO2
TiO2
ZrO(NO3)2

Prefilm

Fracture Time

Max. Stress

Elongation(%)

IGSCC%

5-2 300ppb 10ppb SSRT

5-6 300ppb 25ppb SSRT

Time to
fracture(hr)

Max.
Stress(MPa)

Elongatio
n
(%)

IGSCC
(%)

Prefilm

320

175

11.15

29

ZrO2-150

341

180

11.77

23

339

180

11.79

21

ZrO(NO 3)2-150

56

TiO 2-150

345

186

11.92

400

18

100
ZrO(NO 3)2

350
300

ZrO2

TiO2

Type304SS
[O2]dis:300ppb
[H2]dis :25ppb

Prefilm

80

200
Prefilm

-1

60

ZrO(NO 3)2
TiO 2
ZrO

hr, MPa

-7

288 C Strain rate=1.67*10 S

IPC

250

40

150
Prefilm

100
50
0

Prefilm

Fracture Time

ZrO(NO 3)2
TiO2

ZrO(NO 3)2
ZrO2
TiO2

20

ZrO2

Max. Stress

Elongation(%)

IGSCC%

5-3 300ppb 25ppb SSRT

5-4 5-11 prefilmIPC-ZrO2IPC-ZrO(NO 3)2

IPC-TiO 2
SEM
5-4(c) 5-7(c)
57

IGSCC

304
IGSCC

58

(a)

(b)

(c)
5-4 prefilm 300ppb 10ppb SSRT
(a)IGSCC(b)(c) SEM

59

(a)

(b)

(c)
5-5 IPC-ZrO2 300ppb 10ppb SSRT
(a)IGSCC(b)(c) SEM

60

(a)

(b)

(c)
5-6 IPC- ZrO(NO 3)2 300ppb 10ppb
SSRT (a)IGSCC(b)(c) SEM

61

(a)

(b)

(c)
5-7 IPC- TiO 2 300ppb 10ppb SSRT
(a)IGSCC(b)(c) SEM

62

(a)

(b)

(c)
5-8 prefilm 300ppb 25ppb SSRT
(a)IGSCC(b)(c) SEM

63

(a)

(b)

(c)
5-9 IPC- ZrO2 300ppb 25ppb SSRT
(a)IGSCC(b)(c) SEM

64

(a)

(b)

(c)
5-10 IPC- ZrO(NO 3)2 300ppb 25ppb
SSRT (a)IGSCC(b)(c) SEM

65

(a)

(b)

(c)
5-11 IPC- TiO 2 300ppb 25ppb SSRT
(a)IGSCC(b)(c) SEM

66

5.2
ECP
5-125-13
5-12 ECP ECORRA
ECORRB 5-13
ECP ECORRA ECORRB

5.2.1 ECP
5-14
ECP 100ppb 1000ppb
Prefilm
ECP 300ppb 1000ppb Prefilm
ECP 304 IGSCC
(Ecrit ) -230 mVSHE Prefilm ECP
300ppb -50 mV SHE 1000ppb 50 mV SHE
ECP -150 mVSHE 20 mVSHE ECP
ECP
200ppb Prefilm ECP -130 mV SHE ECP

67

 IGSCC -230 mV SHE 100ppb

Prefilm ECP -230 mVSHE
-230 mVSHE-320 mVSHE ECP
-230 mVSHE
ECP ECP
ECP ECP

5.2.2 10ppb ECP

10ppb ECP 5-15
ECP ECP
1000ppb500ppb300ppb
0.320.160.53 1
1000ppb Prefilm ECP 20 mVSHE ECP
-50 mVSHE -25 mVSHE 500ppb Prefilm ECP
-30 mVSHE ECP -120 mVSHE -80 mVSHE
300ppb Prefilm ECP -100 mVSHE
ECP -200 mVSHE -180 mVSHE Prefilm
10ppb ECP -230
mVSHE 304 IGSCC

68

 10ppb IGSCC
IGSCC

5.2.3 25ppb ECP

25ppb
ECP 5-16 1000ppb500ppb
300ppb 0.40.81.3
1000ppb Prefilm ECP -70 mVSHE ECP
-170 mVSHE -140 mVSHE 500ppb Prefilm
ECP -123 mVSHE ECP -210 mVSHE -190 mVSHE
1000ppb 500ppb ECP
-230mVSHE 300ppb Prefilm ECP
-180 mVSHE ECP -300 mVSHE -280 mVSHE
Prefilm ECP -230mVSHE
-230mVSHE IGSCC Prefilm ECP
100mVSHE

300ppb
IGSCC ECP 304

69

IGSCC 50 mVSHE
IGSCC ECP SSRT
ECP ECP
-230mVSHE SSRT IGSCC

5.2.4 50ppb ECP

ECP 5-17
1000ppb500ppb300ppb 0.81.6
2.7 1000ppb Prefilm
ECP -130 mVSHE -230 mVSHE
ECP -250 mVSHE -220 mVSHE
500ppb Prefilm ECP -210 mVSHE
ECP -330 mVSHE -290 mVSHE
300ppb Prefilm ECP
-230mVSHE-260mVSHE -410 mVSHE -360 mVSHE
ECP 100mVSHE
IGSCC ECP
ECP

70

 ECP
ECP
IGSCC

5-12 ECP

5-13 ECP

71

D.H 0ppb
Prefilm
IPC-ZrO2
IPC-ZrO(NO3)2
0
IPC-TiO2
Zr
-100
100

ECP(mVSHE)

-200
-300
-400
-500
-600
-700
0

200

400

600

800

1000

D.O concentration[ppb]

5-14
ECP

D.H 10ppb
Prefilm
IPC-ZrO2
IPC-ZrO(NO3)2
0
IPC-TiO2
Zr
-100
100

ECP(mVSHE)

-200
-300
-400
-500
-600
-700
0

200

400

600

800

1000

D.O concentration[ppb]

5-15 10ppb
ECP

72

D.H 25ppb
Prefilm
IPC-ZrO2
IPC-ZrO(NO3)2
0
IPC-TiO2
Zr
-100
100

ECP(mVSHE)

-200
-300
-400
-500
-600
-700
0

200

400

600

800

1000

D.O concentration[ppb]

5-16 25ppb
ECP

D.H 50ppb
Prefilm
IPC-ZrO2
IPC-ZrO(NO3)2
0
IPC-TiO2
Zr
-100
100

ECP(mVSHE)

-200
-300
-400
-500
-600
-700
0

200

400

600

800

1000

D.O concentration[ppb]

5-17 50ppb
ECP

73

5.3
5.3.1 AES
AES maps
5-18 x-(x-ray
maps)

Zr Ti
Zr Ti 5-19
AES Zr Ti
Zr Ti
Zr Ti
Auger Zr (~147 eV)

74

 5-18 AES () Zr, Ti maps ()

75

IPC- ZrO2

IPC- ZrO(NO 3)2

IPC- TiO 2
5-19 AES

76


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81