Oxidation Behavior of Zr-Nb Alloys at 973-1273 K in Air

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1043-T09-01

Oxidation behavior of Zr-Nb alloys at 973-1273 K in air T. Arima*), K. Miyata, K. Idemitsu and Y. Inagaki

© 2008 Materials Research Society Department of Applied Quantum Physics and Nuclear Engineering, Faculty of Engineering, Kyushu University, 744 Motooka, Fukuoka 819-0395, Japan E-mail*): [email protected]

2007 MRS Fall Meeting, Nov. 26-30, 2007, Boston, MA (T. Arima)

1

Introduction

I Introduction

Background •

Zr-Nb alloy has been extensively studied from the aspect of thermal treatment, chemical composition and irradiation effects, etc.



For the safe management of fuels, corrosion behaviors under accident condition, e.g. LOCA, should be investigated.

© 2008 Materials Research Society

Objective

To investigate oxidation behaviors of Zr-Nb alloys under the condition of high temperatures (rapid annealing: ~1000 K/120 s, 973-1273 K) and dry air.

2

Materials

II Experimental

Element [wt%] Alloy

Sn

Fe

Cr

O

Zr

Zry-4

1.27

0.11

0.11

0.14

bal.

Nb

O

N

H

Zr

Zr-2.5Nb

2.46

0.090

0.0022

0.0034

bal.

Zr-4Nb

3.93

0.088

0.0025

0.0036

bal.

Zr-6Nb

5.89

0.087

0.0020

0.0033

bal.

Zr-10Nb

9.94

0.085

0.0023

0.0051

bal.

© 2008 Materials Research Society Zr-1Nb 0.99 0.090 0.0020 0.0032 bal.

α-Zr

α-Zr + β-Zr

3

Measurements

II Experimental

Thermo-gravimetry (TG) •

Weight gain due to oxidation was measured by Cahn-2000 micro-balance.



Oxidation tests were performed under flowing dry air at 973-1273 K.

X-ray diffractometry (XRD) •

X-ray diffraction patters from as-received metal and oxidized sample were

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measured by Shimadzu XD-D1. •

All measurements were done at room temperature.

Electron-prove micro-analysis (EPMA) •

Distribution of elements, Nb, Zr and O, were investigated by EPMA-1600 .



Cross sectional view of oxide film on metal was observed.

4

Oxidation in dry air

III Results and discussion

• Parabolic rate law dominates oxidation kinetics at high T and P(O2).

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kinetic transition (parabolic → linear)

5

Weight gain vs. Nb content

III Results and discussion

• Weight gain, δw: At low T, δw is small for low Nb content, and at high T, δw is small for Zr-2.5Nb.

© 2008 Materials Research Society

1273K, air

6

Rate constant for oxidation

III Results and discussion

• Parabolic rate constant, Kp: At low T, Kp is small for low Nb content, and at high T, Kp is small for Zr-2.5Nb. Q ~ 120 kJ/mol

• Activation energy, Q: Q is almost independent on Nb content, and at higher T, smaller Q can be observed.

© 2008 Materials Research Society Q ~ 150 kJ/mol

For samples undergoing rate transition, only pretransition data (parabolic part) was used to obtain Kp. 7

X-ray diffraction from oxide film Oxide film formed on Zr-1Nb alloy consists of m-and t-ZrO2.

III Results and discussion

On the other hand, oxide film formed on Zr-10Nb alloy consists of m-ZrO2 and Zr-Nb oxide compound.

© 2008 Materials Research Society Other peaks : monoclinic

1273K, air

Other peaks : mo