THE SIMULTANEOUS EFFECT OF AGEING AND WATER ENVIRONMENT

ON SUBCRITICAL CRACK GROWTH AND FRACTURE BEHAVIOUR OF

10GN2MFA LOW ALLOY STEEL

Karel MATOCHA
VÍTKOVICE-Research & Development, Ltd., Ostrava, Czech Rep.
František CIKRYT
VÍTKOVICE HEAVY MACHINERY,a.s., Ostrava, Czech Rep.

ABSTRACT

The effect of temper and strain ageing on fracture behaviour and

susceptibility to environmentally assisted cracking of 10GN2MFA steel in
high temperature water was studied. The dominant mechanisms of
subcritical crack growth in water environment at temperatures ranging from
60oC to 290oC was investigated. The results obtained showed, that the
reversed temper embrittlement affects the subcritical crack growth only in
water environment at low water temperatures.

INTRODUCTION

Material properties of safety related components of WWER 1000 steam

generator (SG) may be significantly changed during the service life by ageing.
At sealing of heat exchange tubes into collector body ,using explosive
and/or hydraulic expansion technology, a part or even the entire volume of a
material between holes is exposed to plastic deformation. Due to the fact the
collector body of WWER 1000 SG is made from 10GN2MFA low alloy steel
the strain ageing could occur in these regions.
It is also well known that the toughness of Ni containing low alloy
steels can be severaly reduced by the segregation and build up of residual
impurity elements, such as S,P,Sb,Sn, when the steel is tempered in, or
slowly cooled through the temperature range 300 to 550oC. The result of this
embrittlement is generally brittle fracture along prior austenite grain
boundaries without loss in tensile properties.
The present study was aimed to examine how the strain ageing and
reversed temper embrittlement, simulated by stepcooling ( slow stepwise
cooling from 595oC), affect the subcritical crack growth in 10GN2MFA low
alloy steel in water environment at temperatures ranging from 60oC to
290oC.

BACKGROUND

The subcritical crack growth in ductile alloy/water environment

systems is governed by a complex interaction of material, environment and
loading factors. Due to electrochemical reactions occuring at the crack tip
two main mechanisms (anodic dissolution and/or hydrogen embrittlement)
can be responsible for environmentally controlled crack advance in water

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environment under static or cyclic loading [1]. These two mechanisms can
operate simultaneously because hydrogen is produced as a consequence of
hydrolysis of Fe2+ ions, it means as a result of crack tip anodic dissolution.
Which of the two mechanisms is a dominant one depends on water
temperature, water chemistry, material properties (chemical composition,
structure, yield point) and loading conditions.
There is a lot of experimental evidence the anodic dissolution
mechanism is the dominante cause of environmentally controlled crack
advance under static and/or cyclic loading at water temperature higher than
250oC.

modified anodic dissolution

da/dN [mm/cycle]

model

air
air
water
water

Fig.1 Fatigue crack growth behaviour at 290oC. The effect of cyclic

frequency in aerated water environment.

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 Fig.1 summarizes the results of fatigue crack growth behaviour of
10GN2MFA steel in air and aerated water environment at 290oC.
Experimental data fit very well with modified anodic dissolution/film rupture
model which uses quantitative evaluation of striation spacings for
determination of the crack tip strain rate [2].

10GN2MFA

10 -2

10µmm

ASME, Sec. XI, App.A

10 -3
da/dN [mm/cycle]

0 2 <15ppb
0 2 = 8ppm

10 -4 air 295°C R = 0,5; f = 0,03 Hz

environment: water
air 25°C temp: 295°C; pH = 9,8
air 295°C

10 -5
10 15 20 25 30 35
∆K [MPa1/2]

Fig.2 Effect of oxygen content on fatigue crack growth behaviour of

10GN2MFA steel in high temperature water

Fig.2 summarizes the results of fatigue crack growth behaviour of

10GN2MFA steel in aerated and deaerated water environment at 295oC [3].
Fractographically, cyclic loading in high temperature water produced
features very similar to those obtained in air at 295oC. Fracture surfaces
showed ductile transgranular striations covering large areas and very
pronounced transverse microcracks. There was no evidence of any brittle

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fracture mode. Striation spacings were matched with macroscopic crack
growth measurements. Changes in the oxygen level produced a marked
effect not only on growth rates, but also on striation spacings.
Fig.3 shows the effect of corrosion potential (dissolved oxygen level) on
susceptibility of the studied steel to SCC in demineralized water environment
at 289oC.

10GN2MFA
demineralized water : t = 289°C
Constant displacement test
C(T) (B = 11 mm; W = 50 mm)

oxygen bubbling oxygen purging by nitrogen bubling

25,0 2700

ECP = -0,24 VSHE

crack length [mm]

24,5 ECP = +0,062 VSHE 2600

load [kp]
da/dt = 4,6.10-5 mm/s

24,0 2500

ECP = 0,012 VSHE

ECP = -0,306 VSHE

23,5 2400
4 8 12 16 20 24

time [hour]

Fig.3 The effect of corrosion potential (ECP) on SCC in pure water

environment at 289oC.

C(T) specimen was loaded at ECP = -0,306 VSHE up to K = 105 MPa.m1/2.

Under these conditions no subcritical crack growth was observed. The test
was stopped and under conditions of constant displacement, increasing ECP
by oxygen bubling, the stable crack was started to grow at ECP = 0,012 VSHE
(see Fig.3). In a short time the crack growth rate reached the value of da/dt =

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4,6.10-5 mm/s. The crack growth rate decreased after lowering ECP by
nitrogen bubling and at ECP = -0,24 VSHE the growing crack stopped.
At water temperatures lower than 250oC the detrimental effect of water
environment has been observed as well [4,5].However due to significante
changes in the morphology of crack advance, mainly under cyclic loading
conditions, the environmentally controlled crack advance is often attributed
to hydrogen embrittlement mechanism.
Some ideas concerning the above mentioned mechanisms are
presented in the following text to explain the results of subcritical crack
growth behaviour of 10GN2MFA steel in as received condition, in the state
after strain ageing simulated by 5% plastic deformation followed by
tempering at 250oC for 2 hours and in the state after reversed temper
embrittlement simulated by stepwise cooling from 595oC.

TEST MATERIAL

The testing material was cut off the collector body made in
VÍTKOVICE, J.S.C. from the low alloy 10GN2MFA steel forging. The chemical
composition and tensile properties of the studied structure states at room
temperature are summarized in Tab.I and II respectively.

Tab. I Chemical composition of 10GN2MFA steel under investigation (wt.%)

C Mn Si Ni Cr Mo V P S Cu
0,11 0,97 0,24 1,97 0,21 0,46 0,03 0,009 0,007 0,07

Tab. II Tensile properties of studied structure states at room temperature

Structure Yield Tensile Elongation Reduction of
state strength strength area
[MPa] [MPa] [%] [%]
As received
condition 532 631 25,0 69
After step
cooling 547 647 25,2 74
After strain
ageing 742 742 12,4 66

RESULTS AND DISCUSSION

Tab.II shows the step cooling had no detrimental effect on tensile

properties at laboratory temperature. However severe loss of impact
toughness was observed after this heat treatment. This is a consequence of
phosphorus segregation to prior austenite grain boundaries because the loss
of impact toughness has been accompanied by significante occurence of
intergranular fracture mode.
However both the lower grain boundary strength caused by step
cooling procedure and the significante change of tensile properties caused by
strain ageing had no effect on fatigue crack growth behaviour in air at

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laboratory temperature.It can be explained by experimentally veryfied fact
that the responce of 10GN2MFA steel to reversed strain cycling in all
structure states investigated is practically equal after 10 to 100 cycles. Due
to the fact that the radius of reversed plastic zone, within the studied range
of ∆K, is larger by an order of magnitude than the increment of crack length,
the strain ageing cannot affect the kinetics of fatigue cracks. Fields of
striations and the occurence of transverse microcracks were found to be the
typical microfractographic features [3,6].
Fatigue crack growth behaviour of 10GN2MFA steel in water
environment at temperatures 60oC and 290oC, both for as received condition
and for condition after strain ageing, are illustrated in Fig.4 and Fig. 5.

10GN2MFA
da/dN [mm/cycle]

air

as received cond.

εpl=5%+250°C/2h

aerated distilled water 60°C

sin, f = 1Hz, R = 0,5

∆K [MPa m1/2]

Fig. 4 The effect of strain ageing on fatigue crack growth behaviour in

aerated water at 60oC.

The strain ageing was found to have no effect on the kinetics of fatigue
cracks in water environment at both temperatures too. However
fractographic observations of the fracture surfaces proved that the

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enhancement of fatigue crack growth rate in water environment at 60oC can
be attributed to hydrogen embrittlement of material ahead of the crack tip.
Both the fields of fatigue striations and the areas of transgranular quasi-
cleavage fracture were found only on the fracture surfaces of test specimens
tested in water environment at 60oC. The amount of quasi-cleavage has
increased with increasing ∆K and at ∆K = 26 MPa.m1/2 was equal to
approximately 50%.

10GN2MFA
10-2 f = 0,030 Hz, R = 0,5 , t = 290oC
3, 07
-8 ∆K
(da/dN) INERT. = 9,74.10 [mm/cycle; MPa.m1/2]
10 -3 2,88 − R
O2 = 8000 ppb; S = 0,007%
da/dN [mm/cycle]

10-4

10-5

10-6
{ as received condition
z 5% def. + 250°C/2h
10-7

10-8
101 102
∆K [MPa.m1/2]
Fig. 5 The effect of strain ageing on fatigue crack growth behaviour in
aerated water environment at 290oC.

The effect of step cooling on fatigue crack growth behaviour in aerated

water environment at 60oC and 290oC is shown in Fig.6 and Fig.7. After step
cooling besides the quasi-cleavage fracture mode, the intergranular facets
were observed on fracture surfaces of test specimens cycled at 60oC. In this
case the effect of water environment on fatigue crack growth behaviour was
found to be more pronounced mainly at the lowest ∆K investigated (see
Fig.6).The amount of intergranular fracture (11%), observed at the lowest ∆K
,was decreased with increasing ∆K.
However no quasi-cleavage and intergranular fracture mode was
observed on fracture surfaces of test specimens after step cooling tested in
oxygenated water at 290oC. Fig. 7 shows that these experimental data fit also
very well with anodic dissolution/film rupture model.
All these observations suggest that hydrogen embrittlement could be
responsible for increased fatigue crack growth rates in water at 60oC.
Thermodynamic calculations show that trapping sites like dislocation cores

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 10GN2MFA
HT: step cooling from 595°C
R = 0,5; sin; f = 10Hz

da/dN [mm/cycle]

air - as received
condition

enviroment temp. f [Hz]

air 20°C 10
water 60°C 1

∆K [MPa m1/2]

Fig. 6 The effect of step cooling on fatigue crack growth behaviour in air and
water environment at 60oC.

and grain boundaries should have little or no effect on the hydrogen

solubility in iron at about 230oC for a trap density about 1017 cm-3 [7]. It
means, this temperature could be the crossover point between the
dominance of hydrogen embrittlement and anodic dissolution mechanisms
for low alloy steel under investigation. This hypothesis can be supported by
the results of fatigue crack growth rate measurements carried out in water at
100oC and 200oC [4] and results of slow strain tests in a water environment
at temperatures 100oC, 150oC, 200oC, 250oC and 290oC [5].

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 10GN2MFA, HT: Steep cooling,
aerated woter R=0,5, f=1Hz, sin

modified anodic
dissolution model
da/dN [mm/cycle]

air; 20°C

∆K [MPa m1/2]
Fig. 7 The effect of water temperature on fatigue crack growth behaviour in
10GN2MFA steel after step cooling.

CONCLUSIONS

From the results summarised in this study it follows that:

1. Reversed temper embrittlement simulated by stepwise cooling from

595oC had no effect on tensile properties of 10GN2MFA low alloy steel
but caused severe loss in impact toughness.
2. Neither temper ageing nor strain ageing (simulated by 5% plastic
deformation+250oC/2hours) affected the fatigue crack growth behaviour
in air.
3. The strain ageing did not affect the enhancement of fatigue crack growth
rate in aerated water environment both at 60oC and 290oC compared
with that in air.

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4. The enhancement of fatigue crack growth rate in water at 60oC,
compared with that in air, was attributed mainly to hydrogen
embrittlement of material ahead of the crack tip.
5. Simultaneous effect of reversed temper embrittlement and hydrogen
embrittlement pronounced the effect of water environment at 60oC on
fatigue crack behaviour mainly at low values of ∆K.
6. Anodic dissolution at the crack tip and hydrogen embrittlement of
material ahead of the crack tip are the main mechanisms responsible
for enhanced fatigue crack growth rates and subcritical crack growth
due to SCC in water environment. The temperature of 200oC seems to
be the crossover point between the dominance of hydrogen
embrittlement and anodic dissolution mechanism for low alloy steel
under investigation.

REFERENCES

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