corrosion resistance of al-fe-alloy-coated steel, refractory ......result- refractory metals c o2 =...

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1 Minoru Takahashi, Abu Khalid Rivai Research Laboratory for Nuclear Reactors Tokyo Institute of Technology, Japan Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory Metals and Ceramics in Lead-Bismuth at 700ºC Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory Metals and Ceramics in Lead-Bismuth at 700ºC

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Page 1: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

1

Minoru Takahashi, Abu Khalid Rivai

Research Laboratory for Nuclear ReactorsTokyo Institute of Technology, Japan

Corrosion Resistance of Al-Fe-alloy-coated Steel,

Refractory Metals and Ceramics in Lead-Bismuth at 700ºC

Corrosion Resistance of Al-Fe-alloy-coated Steel,

Refractory Metals and Ceramics in Lead-Bismuth at 700ºC

Page 2: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

2

Motivation

Structural materials: 400-550 ºCHigh Cr F-M steels (with Si and Al addition)

Cladding materials: 650-700 ºCHigh Cr F-M steels with Si and Al additionsAl-Fe-Surface coated steelsRefractory metalsCeramics

High boiling points of lead alloys can provide high temperature reactor with thermal efficiency higher than 40%.

Candidate materials compatible with lead alloys

Page 3: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

3

Materials CompatibilityAustenitic steels SS316, SS316FR poor

Steels12Cr steels10-18Cr steels with Si and Al addition

SUH3, NTK04L, Recloy10, SUS430 excellent

Al-alloyed surface (GESA) ODS locally goodRefractory metalsCeramics

W, Mo excellent

HCM12A, etc. good

SiC, Si3N4 excellent

Flowing fluid: Pb-Bi eutectic (LBE)Temperature: 550°CVelocity: 1 or 2 m/sExposure time: 1,000 or 2,000 hrsOxygen concentration: 10-8-10-6 (wt%)

Results of previous corrosion tests

Page 4: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

4

Purpose

To investigate the compatibility of materials in stirred LBE at 700 ºC

Steels: High Cr steels, Al-Fe-coated onesCeramics: SiC, Ti3SiC2,

SiC/SiC compositesRefractory metals: W, Mo, Nb

Page 5: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

5

Test apparatus

P

Digital

F

FV1

V2V3

V4

V5

V8

V10

V6

V7

ElectrometerPP

Digital Controller

FF

FFV1

V2V3

V4

V5

V8

V10

V6

V7

Steam Generator

Moistureatmosphere

Exhaust NozzleInjection Nozzle

Ar + H2

Ar

Specimens

Page 6: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

6Specimens

Thermocouple

Alumina Crucible

Oxygen Sensor

LBE

Mo Wire

Injection Nozzle

72 mm

100 mm

Corrosion test section

Ceramic

340 mm

Page 7: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

7

Experimental conditions

Run No. 1 No. 2Materials STBA26,

SiC/SiCcomposites

NTK04L, SUS316FR Recloy10, SUS430, Al-Fe-

coated steel, W, Mo, Nb, SiC, Ti3SiC2

Oxygen concentration (wt%) ~6.8x10-7 ~5x10-6

Injection Gas Ar Ar+H2 (3%) and Ar

Type of Sensor Y2O3-ZrO2

Temperature of LBE (ºC) 700Immersion time (hr) 1,000

Page 8: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

8

Al-Fe coating (thickness: 21.45µm)

Target (Al) Target (SUS304)

Bulk Material

Moving Magnet Source

e- e-kinetic energy

Ar Ar

Unbalanced Magnetron Sputtering(UBMS)

Page 9: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

9

Unbalanced Magnetron Sputtering(UBMS)

Specimens

Page 10: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

10

Oxygen concentration

200 300 400 500 600 700-350

-300

-250

-200

-150

-100

0.01

0.1

(1/3)Cr 2 O 3

(1/4)Fe 3 O 4

H 2 O

NiO

PbO

(1/3)Bi 2 O 3

1.0

1010-8

10-7

10-6

10-5

10-4

10-3

P H2 /P H2O

C (wt.%)

Oxygen potential in injected gas (1/2)RT ln P O2

ΔG

o,

Δ

GO

x,

(1/2

)RT

lnP

O2

(kJ/

g at

mO

)

Temperature (°C)

Oxygen potential in Pb-Bi Δ G Ox

Oxygen potentials of oxides Δ G o

5 x 10-6 wt%6.8 x 10-7 wt%

Page 11: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

11

CO2 = 5 x 10-6 wt.% (NTK04L, SUS316FR)CO2 = 6.8 x 10-7 wt.% (STBA26) 700ºC

High Cr Steels (NTK04L, STBA26, SUS316FR)

resin

40µm

Pb-Bi Penetration NTK04L matrix

Cr

Si

Fe

Pb

Bi

O

resin

40µm

Pb-Bi Penetration NTK04L matrix

Cr

Si

Fe

Pb

Bi

O

Cr

Si

Fe

Pb

Bi

O

6.12 µm

resin

6.12 µm

100µm

Pb-Bi Penetration STBA26 matrix

Cr

Si

Fe

Pb

Bi

O

Cr

Si

Fe

Pb

Bi

O

6.12 µm

resin

6.12 µm

100µm

Pb-Bi Penetration STBA26 matrix

Cr

Si

Fe

Pb

Bi

O

Cr

Si

Fe

Pb

Bi

O

resin

30µm

Pb-Bi Penetration SUS316FR matrix

Fe

Cr

Ni

Pb

Bi

O

resin

30µm

Pb-Bi Penetration SUS316FR matrix

Fe

Cr

Ni

Pb

Bi

O

NTK04L 17.8Cr-0.4Si-3.34Al

STBA26 9Cr-0.2Si

SUS316FR 18Cr-12Ni

Page 12: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

12

CO2 = 5 x 10-6 wt%, 700ºC

High Cr Steels (Recloy10 17.7Cr-1Si-0.9Al)

resin

Oxide layer

SUS430 matrix

5.29 µm

3.77 µm

6.94 µm

resin

Oxide layer

SUS430 matrix

5.29 µm

3.77 µm

6.94 µm

5.29 µm

3.77 µm

6.94 µm

resin oxide layer

steel

Cr

resin oxide layer

steel

Cr Si

resin oxide layer

steel

Si

resin oxide layer

steel

10µm10µm

resin oxide layer

steel

Al

resin oxide layer

steel

Al10µm10µm 10µm10µm

6.12 µm

resin

6.12 µm

100µm

Pb-Bi Penetration SUS430 matrix

Cr

Si

Fe

Pb

Bi

Al

6.12 µm

resin

6.12 µm

100µm

Pb-Bi Penetration SUS430 matrix

Cr

Si

Fe

Pb

Bi

Al

Cr

Si

Fe

Pb

Bi

Al

1000h

500h

Page 13: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

13

CO2 = 5 x 10-6 wt%, 700ºC

Bi

High Cr Steels (SUS430 18Cr-0.75Si)

resin

Oxide layer

SUS430 matrix

5.29 µm

6.12 µm

40.0 µm

resin

Oxide layer

SUS430 matrix

5.29 µm

6.12 µm

40.0 µm

5.29 µm

6.12 µm

40.0 µm

resin oxide layer

steel

Cr

resin oxide layer

steel

Cr

10µm

resin oxide layer

steel

Si

resin oxide layer

steel

Si

6.12 µm

resin

6.12 µm

30µm

Pb-Bi Penetration SUS430 matrix

Cr

Si

Fe

Pb

Bi

O

Cr

Si

Fe

Pb

Bi

O

10µm

1000h

500h

Page 14: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

14

Al-Fe-coated (STBA26)

resin

oxide layer STBA26

40 µm

~20 µm

sputtered layer

gold coating

~3.7 µm

resinoxide layer STBA26

40 µm

~20 µm

sputtered layer

gold coating

Fe

Ni

Pb

Bi

Cr

SiAl

O

resinoxide layer STBA26

40 µm

~20 µm

sputtered layer

gold coating

Fe

Ni

Pb

Bi

Cr

SiAl

O

CO2 = 6.8 x 10-7 wt.%, 700ºC

Page 15: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

15

Ceramics1000 hours, CO2 = 5 x 10-6 wt.% (SiC, Ti3SiC2)CO2 = 6.8 x 10-7 wt.% (SiC/SiC composite) , 700ºC

SiC

Ti3SiC2

SiC/SiCcomposite

resin SiC Matrix resin SiC Matrixgold coating

40 µm100 µm

resin SiC Matrix resin SiC Matrixgold coating

40 µm100 µm

resin Ti3SiC2 Matrix resingold coating

30 µm100 µm

Ti3SiC2 Matrixresin Ti3SiC2 Matrix resingold coating

30 µm100 µm

Ti3SiC2 Matrix

5.29 µm

resin

5.29 µm 20.8 µm

33.7 µm

resin

50µm

20.8µm

crackSiC/SiCComposite

33.7µm

100µm

SiC/SiCComposite

5.29 µm

resin

5.29 µm 20.8 µm

33.7 µm

resin

50µm

20.8µm

crackSiC/SiCComposite

33.7µm

100µm

SiC/SiCComposite

Page 16: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

16

Weight Change of Ceramics

-80-70-60-50-40-30-20-10

0102030

SiC Ti3SiC2

Specimens

Wei

ght l

oss (

g/m

2)

SiC/SiCComposite

Page 17: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

17

Result- Refractory Metals

CO2 = 5 x 10-6 wt.%, 700ºC

resin W Matrix resin W Matrix

gold coating

20 µm50 µm

resin W Matrix resin W Matrix

gold coating

20 µm50 µm

resin Mo Matrix resin Mo Matrix

gold coating

20 µm50 µm

resin Mo Matrix resin Mo Matrix

gold coating

20 µm50 µm

resin Nb Matrixadhered Pb-Bi

Pb-Bi penetration

Nb Matrixadhered Pb-Bi

Pb-Bi penetration

40 µm100 µm

resin Nb Matrixadhered Pb-Bi

Pb-Bi penetration

Nb Matrixadhered Pb-Bi

Pb-Bi penetration

40 µm100 µm

W

Mo

Nb

Page 18: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

18

Weight Change of Refractory Metals

-50-25

0255075

100125150175200225250

W Mo Nb

Specimens

Wei

ght l

oss (

g/m

2)

Page 19: Corrosion Resistance of Al-Fe-alloy-coated Steel, Refractory ......Result- Refractory Metals C O2 = 5 x 10-6 wt.%, 700ºC resin W Matrix resin W Matrix gold coating 50 µm 20 µm resin

19

Conclusions

1. Al-Fe-coated steel, W, Mo, SiC and Ti3SiC2exibited good corrosion-resistance in LBE at 700 ºC.

2. Nb exibited poor corrosion-resistance in LBE at 700 ºC.

3. SiC/SiC composite showed that LBE penetrated into the matrix due to high porosity of the material, and a thin crack layer appearedin LBE at 700 ºC.