Creep-fatigue of High Temperature Materials for VHTR: Effect of ...
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INL/CON-11-20780<br />
PREPRINT<br />
<strong>Creep</strong>-Fatigue <strong>of</strong> <strong>High</strong><br />
<strong>Temperature</strong> <strong>Materials</strong><br />
<strong>for</strong> <strong>VHTR</strong>: <strong>Effect</strong> <strong>of</strong><br />
Cyclic Loading and<br />
Environment<br />
ICAPP 2011<br />
C. Cabet<br />
L. Carroll<br />
R. Madland<br />
R. Wright<br />
May 2011<br />
This is a preprint <strong>of</strong> a paper intended <strong>for</strong> publication in a journal or<br />
proceedings. Since changes may be made be<strong>for</strong>e publication, this<br />
preprint should not be cited or reproduced without permission <strong>of</strong> the<br />
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<strong>Creep</strong>-<strong>fatigue</strong> <strong>of</strong> <strong>High</strong> <strong>Temperature</strong> <strong>Materials</strong> <strong>for</strong> <strong>VHTR</strong>:<br />
<strong>Effect</strong> <strong>of</strong> Cyclic Loading and Environment<br />
Proceedings <strong>of</strong> ICAPP 2011<br />
Nice, France, May 2-5, 2011<br />
Paper 11284<br />
C. Cabet<br />
CEA, DEN, DPC, SCCME, Laboratoire d'Etude de la Corrosion Non Aqueuse, F-91191 Gif-sur-Yvette, France<br />
Tel: +33 169 081 615, Fax: +33 169 081 586, Email: celine.cabet@cea.fr<br />
L. Carroll<br />
Idaho National Laboratory<br />
Idaho Falls, ID, USA<br />
R. Madland<br />
Colorado School <strong>of</strong> Mines<br />
Denver, CO, USA<br />
R. Wright<br />
Idaho National Laboratory<br />
Idaho Falls, ID, USA<br />
Abstract – Alloy 617 is the one <strong>of</strong> the leading candidate materials <strong>for</strong> Intermediate Heat<br />
Exchangers (IHX) <strong>of</strong> a Very <strong>High</strong> <strong>Temperature</strong> Reactor (<strong>VHTR</strong>). System start-ups and shut-downs<br />
as well as power transients will produce low cycle <strong>fatigue</strong> (LCF) loadings <strong>of</strong> components.<br />
Furthermore, the anticipated IHX operating temperature, up to 950°C, is in the creep regime so<br />
that creep-<strong>fatigue</strong> interaction, which can significantly increase the <strong>fatigue</strong> crack growth, may be<br />
one <strong>of</strong> the primary IHX damage modes. To address the needs <strong>for</strong> Alloy 617 codification and<br />
licensing, a significant creep-<strong>fatigue</strong> testing program is underway at Idaho National Laboratory.<br />
Strain controlled LCF tests including hold times up to 1800s at maximum tensile strain were<br />
conducted at total strain range <strong>of</strong> 0.3% and 0.6% in air at 950°C. <strong>Creep</strong>-<strong>fatigue</strong> testing was also<br />
per<strong>for</strong>med in a simulated <strong>VHTR</strong> impure helium coolant <strong>for</strong> selected experimental conditions. The<br />
creep-<strong>fatigue</strong> tests resulted in failure times up to 1000 hrs. Fatigue resistance was significantly<br />
decreased when a hold time was added at peak stress and when the total strain was increased. The<br />
fracture mode also changed from transgranular to intergranular with introduction <strong>of</strong> a tensile<br />
hold. Changes in the microstructure were methodically characterized. A combined effect <strong>of</strong><br />
temperature, cyclic and static loading and environment was evidenced in the targeted operating<br />
conditions <strong>of</strong> the IHX. This paper reviews the data previously published by Carroll and coworkers<br />
in references 10 and 11 focusing on the role <strong>of</strong> inelastic strain accumulation and <strong>of</strong><br />
oxidation in the initiation and propagation <strong>of</strong> surface <strong>fatigue</strong> cracks.<br />
I. INTRODUCTION<br />
Alloy 617 is the leading candidate material <strong>for</strong><br />
Intermediate Heat eXchangers (IHX) <strong>of</strong> helium-cooled<br />
Very <strong>High</strong> <strong>Temperature</strong> Reactor (<strong>VHTR</strong>) systems.<br />
Conceptual design requires an outlet temperature <strong>of</strong> greater<br />
than 850°C to efficiently co-generate hydrogen and<br />
electricity, with a maximum expected temperature <strong>of</strong><br />
950°C 1 . The IHX will operate at the reactor outlet<br />
temperature <strong>of</strong> up to 950°C.<br />
Reactor start-ups and shut-downs as well as power<br />
transients will produce low cycle <strong>fatigue</strong> (LCF) loadings <strong>of</strong><br />
components. Furthermore, the anticipated IHX operating<br />
temperature is in the range where creep de<strong>for</strong>mation occurs<br />
so that interaction between a growing <strong>fatigue</strong> crack and the<br />
bulk creep damage, which can significantly increase the<br />
312<br />
<strong>fatigue</strong> crack growth rate, may be one <strong>of</strong> the primary IHX<br />
damage modes. However, in the draft code case that was<br />
developed in the 1980s to have Alloy 617 approved in<br />
ASME Code section III <strong>for</strong> nuclear use at high<br />
temperature 2 , creep-<strong>fatigue</strong> was not sufficiently addressed.<br />
This calls <strong>for</strong> a more complete database <strong>for</strong> creep-<strong>fatigue</strong><br />
behavior <strong>of</strong> Alloy 617; <strong>for</strong> a better understanding <strong>of</strong> the<br />
coupled influence <strong>of</strong> aging, <strong>fatigue</strong>, creep and corrosion;<br />
and <strong>for</strong> a better life prediction <strong>of</strong> components under creep<strong>fatigue</strong><br />
de<strong>for</strong>mation. �<br />
A significant testing program is underway at Idaho<br />
National Laboratory to address the needs <strong>for</strong> codification<br />
and licensing. To reproduce the expected de<strong>for</strong>mation in a<br />
laboratory setting, creep-<strong>fatigue</strong> testing introduces a hold<br />
time in a strain-controlled <strong>fatigue</strong> cycle. Previous work on<br />
Alloy 617 has suggested that a hold time during the tensile
portion <strong>of</strong> the <strong>fatigue</strong> cycle is more damaging 3-5 than<br />
compressive holds or both a tensile and compressive hold.<br />
There<strong>for</strong>e holds at peak tensile strain were investigated.<br />
The helium coolant in the primary circuit <strong>of</strong> a <strong>VHTR</strong><br />
system is expected to contain low levels <strong>of</strong> impurities 6 such<br />
as H2, H2O, CO, CO2, CH4, etc, that can react toward<br />
metallic materials at high temperature. As far as corrosion<br />
<strong>of</strong> Alloy 617 is concerned, the optimum coolant chemistry<br />
will enable the alloy to be oxidized in service <strong>for</strong> the<br />
<strong>for</strong>mation <strong>of</strong> a surface, continuous and dense, chromia<br />
scale which would protect the bulk alloy and has little<br />
influence on the mechanical properties 7 . This corrosion<br />
behavior is similar to oxidation in air at the same<br />
temperature 8,9 . Hence, experiments were per<strong>for</strong>med in air<br />
as well as in controlled <strong>VHTR</strong>-simulated helium to account<br />
<strong>for</strong> any possible environmental effect. To enhance the<br />
understanding <strong>of</strong> creep-<strong>fatigue</strong> de<strong>for</strong>mation mechanisms at<br />
950°C, the <strong>fatigue</strong> and creep-<strong>fatigue</strong> behavior <strong>of</strong> Alloy 617<br />
is presented with systematic microstructure characterization<br />
<strong>of</strong> the alloy surface, the specimen bulk and the vicinity <strong>of</strong><br />
the cracks. This paper reviews the creep-<strong>fatigue</strong> data<br />
presented in two previous references by Carroll et al.<br />
10, 11<br />
with an emphasis on the role <strong>of</strong> inelastic strain<br />
accumulation and the effect <strong>of</strong> oxidation in the initiation<br />
and propagation <strong>of</strong> surface <strong>fatigue</strong> cracks.<br />
II. EXPERIMENTAL<br />
II.A. Material<br />
Cylindrical creep-<strong>fatigue</strong> specimens, 7.5 mm diameter<br />
in the reduced section and a gage length <strong>of</strong> 12 mm, were<br />
machined from Alloy 617 annealed plate; the long axis <strong>of</strong><br />
the specimen aligned with the rolling direction. The<br />
composition <strong>of</strong> the investigated heat <strong>of</strong> Alloy 617 is given<br />
in Table I.<br />
TABLE I<br />
Alloy 617 chemical composition in wt.%.<br />
Ni C Cr Co Mo Fe Al Ti Si Mn Cu<br />
bal 0.08 21.9 11.4 9.3 1.7 1.0 0.3 0.1 0.1 0.04<br />
II.B. Apparatus<br />
Cyclic testing was conducted on servo-hydraulic test<br />
machines in axial strain-control mode in accordance with<br />
the ASTM Standard E606-04 12 . Radio-frequency induction<br />
heating was used to heat the specimens. <strong>Temperature</strong><br />
control was achieved using a combination <strong>of</strong> spot-welded<br />
thermocouples on a shoulder <strong>of</strong> the specimen and a<br />
thermocouple loop at the center <strong>of</strong> the gage section. The<br />
temperature gradient was measured with a specimen<br />
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Paper 11284<br />
instrumented with spot-welded thermocouples along the<br />
gage length and was found to deviate by less than 1%<br />
within the gage section.<br />
For the cyclic tests in controlled chemistry helium, a<br />
servo-hydraulic test frame equipped with a gas-tight<br />
chamber was used. A gas system was developed to feed<br />
<strong>VHTR</strong> simulated coolant to the chamber. It comprises a<br />
manifold containing bottles <strong>of</strong> helium with controlled<br />
partial pressures <strong>of</strong> CO, CH4, and H2; mass flow controller<br />
to regulate the helium flow; and pressure controllers. Small<br />
quantities <strong>of</strong> H2O are added to control the partial pressure<br />
<strong>of</strong> water vapor in the helium flow (P(H2O) as low<br />
as 5μbar). A gas chromatograph and two solid-state<br />
hygrometers record the gas chemistry at the inlet and outlet<br />
<strong>of</strong> the chamber. Feedback is employed on the inlet<br />
hygrometry.<br />
II.C. Testing methods<br />
Fully reversed strain controlled low cycle <strong>fatigue</strong> and<br />
creep-<strong>fatigue</strong> testing was completed on Alloy 617 at a total<br />
strain range <strong>of</strong> 0.3% and 0.6% in air and a simulated<br />
<strong>VHTR</strong> helium at 950°C. A triangular wave<strong>for</strong>m and a ramp<br />
rate <strong>of</strong> 10 -3 /s were used <strong>for</strong> low cycle <strong>fatigue</strong> testing.<br />
<strong>Creep</strong>-<strong>fatigue</strong> testing followed a trapezoidal wave<strong>for</strong>m with<br />
a tensile hold imposed at the maximum tensile strain.<br />
Tensile holds <strong>of</strong> 180, 600, and 1800 sec were investigated.<br />
The number <strong>of</strong> cycles to failure, Nf, is defined as the point<br />
at which the ratio <strong>of</strong> the peak tensile stress to the peak<br />
compressive stress initially deviated from its level slope<br />
and the point at which the ratio was 80% <strong>of</strong> the value at<br />
deviation 12 . Test completion was prior to actual specimen<br />
separation.<br />
For testing in helium, a gas mixture was selected to<br />
roughly simulate the controlled <strong>VHTR</strong> coolant. It contained<br />
50 μbar CO and 350 μbar H2 in addition to approximately<br />
8 μbar H2O at 1.1 bar total helium pressure to be oxidizing<br />
with respect to Alloy 617.<br />
II.D. Specimen characterization<br />
After creep-<strong>fatigue</strong> de<strong>for</strong>mation, the gage sections <strong>of</strong><br />
the de<strong>for</strong>med specimens were cut along the stress axis<br />
through the largest surface crack. The specimen was then<br />
coated with a thin layer <strong>of</strong> gold followed by nickel plating<br />
to ensure retention <strong>of</strong> the surface oxide. The coated<br />
specimens were mounted in phenolic, polished to a mirror<br />
finish, and then etched with a 2% bromine solution in<br />
methanol. Metallurgical evaluation was conducted with<br />
optical microscopy and Field Emission Gun-Scanning<br />
Electron Microscopy (FEG-SEM) equipped with an EDX<br />
spectrometer.
III. RESULTS<br />
III.A. Low cycle <strong>fatigue</strong> behavior<br />
Continuous low cycle <strong>fatigue</strong> (LCF) testing was<br />
completed at 950°C to provide a baseline <strong>for</strong> the creep<strong>fatigue</strong><br />
behavior. Two total strain ranges were investigated,<br />
0.3% and 0.6%, in air and in helium. The number <strong>of</strong> cycles<br />
to failure and the total test time are included in Table II.<br />
TABLE II<br />
Fatigue and creep-<strong>fatigue</strong> tests completed at 950°C and a<br />
strain rate <strong>of</strong> 10 -3 /s.<br />
Strain range<br />
(%)<br />
Hold time<br />
(s)<br />
Environment<br />
Nf (cycle)<br />
Time<br />
(h)<br />
0 air 9641 16<br />
0 air 7133 12<br />
0 air 5867 10<br />
0 air 9000 15<br />
0 helium 8000 13<br />
0 helium 7333 12<br />
180 air 3989 210<br />
180 air 2485 130<br />
0.3<br />
180<br />
180<br />
air<br />
helium<br />
4486<br />
3004<br />
230<br />
155<br />
180 helium 3373 174<br />
600 air 4096 690<br />
600 air 2623 440<br />
600 air 4361 735<br />
600 air 4430 745<br />
600 helium 3130 530<br />
1800 air 4805 2410<br />
1800 air 4650 2330<br />
0 air 1722 6<br />
0 air 1390 5<br />
0 air 1480 5<br />
0.6<br />
180<br />
180<br />
air<br />
air<br />
950<br />
922<br />
51<br />
49<br />
600 air 686 117<br />
600 air 634 108<br />
1800 air 661 333<br />
The peak tensile and compressive stresses observed in<br />
the LCF tests at 0.3% and 0.6% total strain were relatively<br />
symmetrical, i.e. the peak tensile and compressive stresses<br />
were <strong>of</strong> the same magnitude, as shown in Figures 1a and<br />
2a, respectively. Furthermore, a steady state stress was<br />
reached in approximately 10 cycles and remained constant<br />
until macrocrack initiation or just prior to failure. Also,<br />
note that the steady state peak stress in the 0.6% total strain<br />
test was similar in magnitude to the 0.3% total strain test.<br />
This is consistent with the shape <strong>of</strong> the hysteresis loops<br />
shown in Figures 1b and 2b <strong>for</strong> the 0.3% and 0.6% total<br />
strain conditions, respectively. The hysteresis loops were<br />
relatively unchanging <strong>for</strong> cycles 9, 99, and 999 and thus the<br />
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Proceedings <strong>of</strong> ICAPP 2011<br />
Nice, France, May 2-5, 2011<br />
Paper 11284<br />
inelastic strain also did not change significantly as a<br />
function <strong>of</strong> cycle.<br />
III.B. <strong>Creep</strong>-<strong>fatigue</strong> behavior<br />
<strong>Creep</strong>-<strong>fatigue</strong> testing was also conducted at 950°C and<br />
at 0.3% and 0.6% total strains with tensile hold times <strong>of</strong> up<br />
to 1800s. A list <strong>of</strong> the creep-<strong>fatigue</strong> conditions and <strong>fatigue</strong><br />
life is shown in Table II; total test times were as long as one<br />
month.<br />
The peak tensile and compressive stresses are also<br />
shown as a function <strong>of</strong> cycle <strong>for</strong> the creep-<strong>fatigue</strong> tests<br />
(Figures 1a and 2a). The creep-<strong>fatigue</strong> peak stresses versus<br />
cycle pr<strong>of</strong>iles were similar regardless <strong>of</strong> the duration <strong>of</strong> the<br />
tensile hold. The creep-<strong>fatigue</strong> peak stresses versus cycle<br />
pr<strong>of</strong>iles were also relatively symmetric, although the<br />
magnitude <strong>of</strong> the stresses in compression were slightly<br />
greater than in tension. The peak stresses did not achieve a<br />
steady state value, instead the peak stresses slowly<br />
decreased with cycle and had two transition points<br />
following which a more rapid decrease was observed. The<br />
hysteresis loops shown in Figures 1c and 2c illustrate this<br />
cyclic s<strong>of</strong>tening. The loops shown <strong>for</strong> cycles 999 and 499<br />
demonstrated a lower peak stress magnitude versus cycle<br />
99, although the width <strong>of</strong> the loops at zero stress, the<br />
inelastic strain, did not vary greatly.<br />
III.C. <strong>Creep</strong>-<strong>fatigue</strong> life in air and in helium<br />
Figure 3 and Table II give the cycles to failure <strong>for</strong> LCF<br />
and creep-<strong>fatigue</strong> testing at 950°C in air and in helium.<br />
The continuous cycle <strong>fatigue</strong> lives were longer than<br />
corresponding creep-<strong>fatigue</strong> lifetimes. For example in the<br />
case <strong>of</strong> the 0.3% total strain range, the addition <strong>of</strong> a 180s<br />
hold time reduced the number <strong>of</strong> cycles to failure by a<br />
factor <strong>of</strong> 2. However, the increasing duration <strong>of</strong> tensile hold<br />
did not further decrease the creep-<strong>fatigue</strong> life at least at a<br />
total strain range <strong>of</strong> 0.3%, i.e. the cycle life with a 180s<br />
hold was comparable to the cycle life with a 1800s hold.<br />
The influence <strong>of</strong> the hold duration on the <strong>fatigue</strong> life at a<br />
0.6% total strain still needs to be ascertained.<br />
For continuous <strong>fatigue</strong> testing as well as <strong>for</strong> creep<strong>fatigue</strong><br />
at 950°C, the cycle life <strong>of</strong> Alloy 617 in air and in<br />
<strong>VHTR</strong> simulated helium was within the same scatter band,<br />
as shown in Figure 3. Similar peak tensile stresses were<br />
also observed in air and impure helium (see Figure 4).<br />
Again in continuous cycle <strong>fatigue</strong>, the peak stresses<br />
achieved a steady state value while cyclic s<strong>of</strong>tening was<br />
observed in creep-<strong>fatigue</strong>.
a.<br />
b.<br />
c.<br />
Fig. 1. LCF and creep-<strong>fatigue</strong> tests in air at 950°C and a<br />
0.3% total strain: a) peak tensile and compressive stresses as a<br />
function <strong>of</strong> cycle; b) hysteresis loops <strong>for</strong> a LCF test and c)<br />
hysteresis loops <strong>for</strong> a 60s hold creep-<strong>fatigue</strong> test.<br />
315<br />
a.<br />
b.<br />
c.<br />
Proceedings <strong>of</strong> ICAPP 2011<br />
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Paper 11284<br />
Fig. 2. LCF and creep-<strong>fatigue</strong> tests in air at 950°C and a<br />
0.6% total strain: a) peak tensile and compressive stresses as a<br />
function <strong>of</strong> cycle; b) hysteresis loops <strong>for</strong> a LCF test and c)<br />
hysteresis loops <strong>for</strong> a 60s hold creep-<strong>fatigue</strong> test.
Cycle to failure<br />
10000<br />
1000<br />
100<br />
0.3% total strain in air<br />
0.3% total strain in helium<br />
0.6% total strain in air<br />
0,01 1 100 10000<br />
Hold time (s)<br />
Fig. 3. Cycles to failure as a function <strong>of</strong> hold time <strong>for</strong> LCF<br />
and creep-<strong>fatigue</strong> tests in air and in helium at a 0.3% and 0.6%<br />
total strain.<br />
a.<br />
b.<br />
Fig. 4. Peak tensile stresses as a function <strong>of</strong> cycle in air and<br />
in helium at a 0.3% total strain <strong>for</strong> a) LCF and cb) reep-<strong>fatigue</strong><br />
with a 180s hold time.<br />
Typical stress relaxation curves at mid-life are shown<br />
in Figure 5 <strong>for</strong> creep-<strong>fatigue</strong> tests with a hold time up to<br />
1800s with a 0.3% and 0.6% total strain. During the hold<br />
period at constant strain, the stress relaxed at the same rate<br />
<strong>for</strong> all hold durations: it initially decreased rapidly and was<br />
almost completely relaxed after approximately 180s into<br />
the hold.<br />
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Paper 11284<br />
Fig. 5. Stress relaxation at mid-life during the tensile hold<br />
<strong>for</strong> creep-<strong>fatigue</strong> specimens tested in air a) at 0.3% total strain<br />
with a 180s, 600s, and 1800s hold time and b) at 0.6% total strain<br />
with a 180s, and 600s hold time.<br />
III.D. Failure mode<br />
No noticeable difference was observed in specimen<br />
cracking after cyclic testing in air and in helium. Hence in<br />
the following, results from both environments are presented<br />
together.<br />
In continuous cycling tests, the primary crack (most<br />
likely initiated and) propagated in a predominantly<br />
transgranular manner, perpendicular to the stress axis.<br />
Figure 6 shows longitudinal cross sections through the<br />
specimen gage after LCF. The edges <strong>of</strong> the cracks were<br />
slightly oxidized and there was little indication <strong>of</strong> an oxide<br />
having <strong>for</strong>med on the surface <strong>of</strong> the specimens. A few wide<br />
but short intergranular secondary cracks were observed<br />
perpendicular to the stress axis in the specimens tested at a<br />
0.6% total strain.<br />
The addition <strong>of</strong> a hold time resulted in multiple larger<br />
or primary cracks originating from the specimen surface as<br />
well as an evolving microstructure, particularly at the<br />
specimen surface. For the specimens tested in creep<strong>fatigue</strong>,<br />
all <strong>of</strong> the grain boundaries close to the specimen
surface and perpendicular to the stress axis were oxidized<br />
(the intergranular oxide was mainly Al-rich). A majority <strong>of</strong><br />
these surface internal oxides have initiated intergranular<br />
cracks (after opening, the edges <strong>of</strong> these small secondary<br />
cracks have oxidized and eventually the cracks were fully<br />
filled by the Cr-rich oxide) as can be seen in Figure 7a. It is<br />
difficult to determine on the initiation mode <strong>of</strong> the primary<br />
crack (or cracks) because <strong>of</strong> the evolving microstructure at<br />
the surface and surrounding the cracks. However, based on<br />
the many shorter secondary cracks which started at<br />
oxidized grain boundaries, it is likely that the primary<br />
cracking also initiated intergranularly.<br />
a.<br />
Fig. 6. Cracking in continuously cycled specimens de<strong>for</strong>med<br />
in air at a) a 0.3% total strain and b) a 0.6% total strain. The<br />
stress axis is horizontal and in the plane <strong>of</strong> the page.<br />
The crack propagation was intergranular. In Figure 7a,<br />
the primary crack was open and an oxide, rich in Cr and<br />
containing Ti, has <strong>for</strong>med along the flanks. Grain<br />
boundaries intersecting with the main crack exhibit fine<br />
carbides and Al-rich precipitates, most certainly alumina.<br />
Figure 7b illustrates oxidation at the crack tip. Alumina was<br />
detected ahead <strong>of</strong> the main crack tip as fine intergranular<br />
veins.<br />
III.E. Surface evolution<br />
The surface microstructure in the specimens cycled in<br />
air was qualitatively similar to those cycled in impure<br />
helium. There<strong>for</strong>e, the results reported in this section do<br />
not differentiate between testing environment. In addition<br />
the microstructure <strong>of</strong> de<strong>for</strong>med specimens was consistent<br />
with statically exposed specimens 8,13 with the exception <strong>of</strong><br />
occurrence <strong>of</strong> secondary and primary cracking.<br />
b.<br />
317<br />
a.<br />
b.<br />
intergranular<br />
crack<br />
Al-rich<br />
precipitates<br />
Proceedings <strong>of</strong> ICAPP 2011<br />
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Paper 11284<br />
hole<br />
Cr-rich oxide<br />
40 µm<br />
100 µm<br />
Fig. 7. Cracking in creep-<strong>fatigue</strong> specimens de<strong>for</strong>med in air<br />
at a 0.3% total strain with a) a 600s hold and b) a 180s hold<br />
(close up <strong>of</strong> the crack tip). The stress axis is horizontal and in the<br />
plane <strong>of</strong> the page.<br />
Figure 7a exemplifies the basic features <strong>of</strong> the surface<br />
evolution:<br />
- A Cr-rich oxide scale has <strong>for</strong>med which covers the<br />
entire surface. Variations in the scale thickness were<br />
related to the total time exposed at 950°C: after<br />
continuous cycle <strong>fatigue</strong>, the oxide was relatively<br />
thin (approximately 2µm), while after creep-<strong>fatigue</strong><br />
de<strong>for</strong>mation a thicker oxide had <strong>for</strong>med (up to<br />
10µm).<br />
- Internal Al-rich oxides, precipitated beneath the<br />
chromia scale and at grain boundaries close to the<br />
surface. In continuously cycled specimens, the<br />
intergranular oxides were thin and finger-like. In<br />
creep-<strong>fatigue</strong> de<strong>for</strong>med specimens, the depth <strong>of</strong><br />
grain boundary oxides was greater, and as<br />
previously explained, some had evolved into<br />
secondary cracks filled with a Cr-rich oxide.
- An area free <strong>of</strong> grain boundary carbides has evolved<br />
in the subsurface. Such a carbide-depletion was also<br />
evidenced in the region surrounding the primary<br />
creep-<strong>fatigue</strong> cracks. Carbide dissolution was<br />
related to the diffusion <strong>of</strong> chromium to the surface<br />
(<strong>of</strong> the specimen or <strong>of</strong> the crack) to <strong>for</strong>m the<br />
chromia scale. Chromium removal then may have<br />
destabilized the grain boundary Cr-rich carbides in<br />
the subsurface area.<br />
III.F. Bulk evolution<br />
For pure <strong>fatigue</strong> specimens (and oxidized coupons<br />
without loading as well), the material bulk was clean from<br />
cracking. On the contrary, cracks were observed in the bulk<br />
<strong>of</strong> the creep-<strong>fatigue</strong> tested specimens. Examples <strong>of</strong> these<br />
cracks are shown in the images in Figure 8.<br />
a.<br />
b.<br />
50 µm<br />
50 µm<br />
Fig. 8. Grain boundary damage observed in the bulk material<br />
<strong>of</strong> specimens de<strong>for</strong>med at a 0.3% total strain range with a) a 180 s<br />
hold in impure helium and b) a 600 s hold in air. The stress axis is<br />
horizontal and in the plane <strong>of</strong> the page.<br />
The cracks were relatively thin and typically followed<br />
grain boundaries perpendicular to the stress axis. Their<br />
length varied, from several micrometers to several grain<br />
diameters in length. In some cases, there were boundaries<br />
with multiple small cracks. Although this type <strong>of</strong> damage<br />
was randomly distributed in the bulk, most <strong>of</strong> the grain<br />
boundaries were completely free <strong>of</strong> cracking and these<br />
intact grain boundaries did not exhibit cavitation and<br />
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instead microscopically appeared free <strong>of</strong> grain boundary<br />
damage (at magnifications <strong>of</strong> up to 100,000 times). The<br />
bulk cracks were absent <strong>of</strong> any oxide and thus it can be<br />
concluded that they were not surface connected and<br />
exposed to the environment.<br />
IV. DISCUSSION<br />
IV.A. <strong>Effect</strong> <strong>of</strong> an air or helium environment<br />
The cycle lives <strong>of</strong> continuous cycle and creep-<strong>fatigue</strong><br />
<strong>of</strong> Alloy 617 in air and in <strong>VHTR</strong> simulated helium were<br />
within the same scatter band at 950°C, as shown in<br />
Figure 3. This tendency is rather consistent with the small<br />
number <strong>of</strong> previous studies on the influence in <strong>fatigue</strong> <strong>of</strong> air<br />
compared to impure helium. Nagato and coworkers 14<br />
observed that the <strong>fatigue</strong> life <strong>of</strong> Hastelloy X, a nickel base<br />
alloy rich in Cr, was longer in impure helium than in air but<br />
the effect <strong>of</strong> environment was less remarkable at<br />
temperatures above 800°C and <strong>for</strong> creep-<strong>fatigue</strong>. At<br />
temperatures <strong>of</strong> 750°, 850° and 950°C, Meurer and<br />
coworkers 5 observed a slight increase in the <strong>fatigue</strong> life <strong>of</strong><br />
Alloy 617 tested in impure helium compared to air at a<br />
total strain <strong>of</strong> 0.3%; this difference was not evidenced at<br />
higher strain ranges. Strizak and coworkers 15 observed that<br />
a helium environment was not detrimental to <strong>fatigue</strong> life <strong>of</strong><br />
Alloy 617 at temperatures <strong>of</strong> up to 704°C and Rao and<br />
coworkers 3 concluded that at 950°C the influence <strong>of</strong><br />
environment, if any, is strongly reduced <strong>for</strong> longer hold<br />
times. In addition to an equivalent <strong>fatigue</strong> life, the<br />
tensile/compressive peak stress versus cycle, the hysteresis<br />
loop, and the stress relaxation during the peak tensile hold<br />
were similar under both atmospheres (see Figure 4). No<br />
difference in the crack initiation behavior, propagation<br />
mode, or oxidation <strong>of</strong> the cracks was evidenced between<br />
the air and impure helium cycled specimens. Finally,<br />
metallurgical characterization <strong>of</strong> the specimens cyclically<br />
de<strong>for</strong>med in air and in helium failed to reveal any<br />
significant differences in the oxidation products or surface<br />
morphology. The corrosion product development and the<br />
surface evolution are consistent with the general corrosion<br />
behavior <strong>of</strong> Alloy 617 under a high temperature oxidizing<br />
environment as is air or controlled <strong>VHTR</strong> helium coolant<br />
(helium with significant water vapor and carbon monoxide<br />
partial pressures at 950°C). In an atmosphere with a<br />
sufficient oxidation potential, Alloy 617 <strong>for</strong>ms a chromia<br />
surface scale and aluminum oxidizes internally 9,13 . These<br />
similarities in the overall behavior <strong>of</strong> the specimens cycled<br />
in air and in simulated impure <strong>VHTR</strong> helium allow <strong>for</strong> the<br />
joint discussion <strong>of</strong> the results <strong>for</strong> both environments<br />
without specific reference to the testing atmosphere.
IV.B. Basis <strong>for</strong> creep-<strong>fatigue</strong> interaction<br />
<strong>Creep</strong>-<strong>fatigue</strong> interaction is a combination <strong>of</strong> creep<br />
damage and <strong>fatigue</strong> damage which accelerates the<br />
de<strong>for</strong>mation process. Typically three types <strong>of</strong> failure are<br />
defined: <strong>fatigue</strong>-dominated, creep-dominated, and creep<strong>fatigue</strong><br />
interaction 16-18 . Fatigue dominated failures are<br />
typically observed at lower to intermediate temperatures<br />
and transgranular crack initiation and propagation is<br />
observed. On the contrary, creep dominated failures occur<br />
at high temperatures and intergranular crack initiation and<br />
propagation with extensive creep cavitation occurs. <strong>Creep</strong><strong>fatigue</strong><br />
interaction is illustrated as mixed-mode crack<br />
propagation and the presence <strong>of</strong> creep cavitation on the<br />
grain boundaries in the bulk material. Cavity <strong>for</strong>mation and<br />
<strong>fatigue</strong> crack initiation and propagation independently<br />
develop, then interaction occurs if one mode accelerates the<br />
other damage process. The creep and <strong>fatigue</strong> failure modes<br />
interact through cavitation accelerating the crack initiation<br />
or propagation process or <strong>fatigue</strong> de<strong>for</strong>mation enhancing<br />
cavitation 18 . Identifying the dominant failure mode and the<br />
influence <strong>of</strong> environment is important <strong>for</strong> life prediction<br />
and modeling ef<strong>for</strong>ts.<br />
On the one hand, the creep-<strong>fatigue</strong> specimens did not<br />
fail in a <strong>fatigue</strong>-dominated manner at 950°C. The primary<br />
crack in the continuously cycled specimens initiated and<br />
propagated in a transgranular manner (<strong>fatigue</strong> dominated<br />
manner). Oxidized grain boundaries were occasionally<br />
present but did not result in specimen failure. For all cases<br />
in creep-<strong>fatigue</strong>, several longer cracks likely initiated and<br />
did propagate intergranularly. Rao and coworkers 3 also<br />
reported transgranular cracking <strong>of</strong> Alloy 617 at 950°C in<br />
<strong>fatigue</strong> cycled specimens and the addition <strong>of</strong> a 60s tensile<br />
hold resulted in the cracking initiating transgranularly and<br />
propagating by a mixed mode. Besides, at lower strain rates<br />
in a helium environment: approximately 10 -4 /s, the crack<br />
propagation mode switched to intergranular.<br />
On the other hand, massive cavitation which would<br />
have caused creep dominated failure was not observed in<br />
any <strong>of</strong> the creep-<strong>fatigue</strong> specimens de<strong>for</strong>med at 950°C with<br />
holds as long as 1800s. Grain boundary cavities were<br />
depicted <strong>for</strong> many alloys in the regime <strong>of</strong> creep-<strong>fatigue</strong><br />
interaction 3,16,18-20 . A detailed assessment correlated the<br />
size and number <strong>of</strong> grain boundary cavities and the<br />
accumulated creep damage <strong>for</strong> 316 stainless steel 16 . It was<br />
also found that a critical amount <strong>of</strong> de<strong>for</strong>mation was<br />
required be<strong>for</strong>e creep cavities nucleated. Recent work by<br />
Lillo and co-workers 21 suggested that significant creep<br />
cavitation did not occur in Alloy 617 until greater than<br />
10% creep strain during creep de<strong>for</strong>mation in the<br />
temperature range from 900°C to 1000°C. Inelastic strain<br />
was evaluated by integrating the stress relaxation data from<br />
Figure 5 [this calculation was done by S. Sham from Oak<br />
Ridge National Laboratory]. The total inelastic strain was<br />
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calculated by integrating the stress relaxation curve at a<br />
mid-life cycle. The accumulated creep strain was estimated<br />
to be less than 2.5% and 0.5% <strong>for</strong> respectively the 0.3%<br />
and the 0.6% total strain tests,. There<strong>for</strong>e, creep cavities<br />
are not expected to be <strong>for</strong>med in the present testing <strong>of</strong><br />
Alloy 617 at 950°C.<br />
IV.C. <strong>Effect</strong> <strong>of</strong> a hold period in tensile strain<br />
Similar to what has been observed <strong>for</strong> stainless steels<br />
and nickel base alloys, the introduction <strong>of</strong> hold times at<br />
peak tensile strain in continuous cycle <strong>fatigue</strong> reduces the<br />
<strong>fatigue</strong> life <strong>of</strong> Alloy 617 (Figure 3). For example at a 0.3%<br />
total strain, the introduction <strong>of</strong> a 180s hold period at peak<br />
tensile strain decreased the life by approximately a factor<br />
<strong>of</strong> 2. A greater decrease in cycles to failure at lower strain<br />
ranges was also observed, consistent with the results on<br />
Nimonic PE-16, a Ni-Cr superalloy 19 .<br />
The drop in cycle life is likely associated with the<br />
change in the cracking mode. The shift in crack<br />
propagation mode from transgranular to intergranular may<br />
be a result <strong>of</strong> grain boundary damage from creep processes<br />
that accelerates intergranular crack propagation (see<br />
paragraph IV.B) but may be also influenced by the<br />
environment accelerating grain boundary crack propagation<br />
and promoting intergranular failure.<br />
Interestingly, the increasing duration <strong>of</strong> the peak<br />
tensile hold at 0.3% total strain did not further decrease the<br />
number <strong>of</strong> cycles to failure; that is to say, the 180s hold<br />
creep-<strong>fatigue</strong> life was similar to that <strong>of</strong> the 1800s hold. The<br />
amount <strong>of</strong> creep damage, estimated by the accumulated<br />
inelastic strain, is relatively similar with increasing hold<br />
periods as the stresses during the tensile hold were almost<br />
completely relaxed by the end <strong>of</strong> the first 180s.<br />
This suggests creep-<strong>fatigue</strong> interaction in the current<br />
testing. Although creep intergranular cavities were not<br />
observed, bulk cracking was evidenced in all <strong>of</strong> the creep<strong>fatigue</strong><br />
de<strong>for</strong>med specimens as illustrated in Figure 8.<br />
Because intergranular crack was not found in the<br />
continuously cycle <strong>fatigue</strong> specimens (or in unloaded<br />
material), it was assumed that bulk cracking was caused by<br />
creep de<strong>for</strong>mation.<br />
The amount <strong>of</strong> bulk material cracking was quantified<br />
to determine if a relationship existed between the duration<br />
<strong>of</strong> the hold time and the amount <strong>of</strong> grain boundary damage.<br />
The total number <strong>of</strong> cracks, total length <strong>of</strong> cracks, and the<br />
average length <strong>of</strong> the cracks were determined <strong>for</strong> a<br />
(0.5mm)² area at five locations, as shown schematically in<br />
Figure 9.<br />
The areas analyzed were 1mm in each direction (in the<br />
plane <strong>of</strong> the page) from the primary crack tip and 3mm in<br />
each direction along the stress axis (in the plane <strong>of</strong> the<br />
page) from the primary crack tip. For all specimens, the<br />
cracking was statistically similar among the five areas and<br />
no general trends were observed. In particular, the amount
or length <strong>of</strong> the bulk cracking did not appear to be related<br />
to location relative to the primary crack. Hence, the<br />
cracking features (number, average length, cumulated<br />
length <strong>of</strong> the cracks) were calculated <strong>for</strong> the all <strong>of</strong> the areas<br />
combined. Figure 10 shows the results graphically as a<br />
function <strong>of</strong> hold time. As mentioned previously, there was<br />
no cracking observed in the continuous cycle <strong>fatigue</strong><br />
specimens. It was also evidenced that increasing hold times<br />
induced relatively similar amounts <strong>of</strong> grain boundary<br />
cracking. Additionally, whatever the environment, air or<br />
impure helium, the material exhibited a similar degree <strong>of</strong><br />
bulk grain boundary cracking.<br />
Fig. 9. Schematic <strong>of</strong> the statistical method used to quantify<br />
damage in the LCF and creep-<strong>fatigue</strong> de<strong>for</strong>med specimens. The<br />
stress axis is horizontal and in the plane <strong>of</strong> the page.<br />
It is believed that creep-<strong>fatigue</strong> interaction may be<br />
caused by bulk cracking accelerating the surface <strong>fatigue</strong><br />
crack propagation. Equivalent creep strain accumulated <strong>for</strong><br />
a 180s hold and a 1800s hold (because <strong>of</strong> the rapid<br />
relaxation) would produce similar amount <strong>of</strong> grain<br />
boundary cracking, resulting in the same reduction <strong>of</strong> the<br />
creep-<strong>fatigue</strong> life. Although the main factor in the drop in<br />
the <strong>fatigue</strong> life when a hold is introduced may be the creep<br />
damage promoting intergranular crack propagation,<br />
oxidation may also play a role.<br />
IV.D. Role <strong>of</strong> oxidation<br />
One faces a challenge in discussing the role <strong>of</strong><br />
environment at elevated temperature. In an ideal case,<br />
comparable creep-<strong>fatigue</strong> testing per<strong>for</strong>med under an inert<br />
atmosphere would be used as a baseline, exemplifying the<br />
effect <strong>of</strong> oxidation on <strong>fatigue</strong> life. However, creep-<strong>fatigue</strong><br />
in inert conditions is not practically achievable at high<br />
temperature.<br />
320<br />
a.<br />
b.<br />
c.<br />
Number <strong>of</strong> cracks<br />
Average length (μm)<br />
Total length (μm)<br />
110<br />
100<br />
90<br />
80<br />
70<br />
60<br />
50<br />
40<br />
35<br />
30<br />
25<br />
20<br />
15<br />
10<br />
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0.3% - air<br />
0.6% - air<br />
0.3% - helium<br />
0<br />
0 500 1000 1500 2000<br />
��������������<br />
Hold Time (sec)<br />
0.3% - air<br />
0.6% - air<br />
0.3% - helium<br />
30<br />
0 500 1000<br />
Hold �������������� time (sec)<br />
1500 2000<br />
2000<br />
1500<br />
1000<br />
500<br />
0.3% - air<br />
0.6% - air<br />
0.3% - helium<br />
0<br />
0 500 1000 1500 2000<br />
��������������<br />
Hold time (sec)<br />
Fig. 10. Grain boundary cracking analysis <strong>for</strong> LCF and<br />
creep-<strong>fatigue</strong> testing in air and in helium; a) total number <strong>of</strong><br />
cracks, b) crack average length, and c) total length.
Exposure at 950°C in vacuum and in (never<br />
completely) pure helium or argon is accompanied by<br />
decarburization. Dissolution <strong>of</strong> intergranular carbides to an<br />
increasing depth fosters grain boundary sliding and the<br />
<strong>for</strong>mation <strong>of</strong> cavities and wedge-cracks in the carbide-free<br />
region 3,18 . These metallurgical instabilities contribute to the<br />
<strong>fatigue</strong> crack initiation and/or growth, and the <strong>fatigue</strong> life<br />
may be significantly lower than observed in air 3 . There<strong>for</strong>e,<br />
characterization <strong>of</strong> the cycled alloy microstructure on the<br />
surface and in the surrounding <strong>of</strong> the cracks will be used to<br />
get an insight <strong>of</strong> the possible role <strong>of</strong> oxidation in the <strong>fatigue</strong><br />
crack initiation and growth.<br />
Close examination <strong>of</strong> cross sections <strong>of</strong> the creep<strong>fatigue</strong><br />
tested specimen revealed that surface grain<br />
boundaries were either cracked or showed precipitation <strong>of</strong><br />
finger-like alumina (see Figure 7a). Intergranular alumina<br />
precipitates are typical <strong>of</strong> Alloy 617 oxidized in air or in an<br />
impure but oxidizing helium (as is the process gas in the<br />
present study): the oxygen potential at the scale/alloy<br />
interface, set by the dissociation <strong>of</strong> chromia, is very low but<br />
high enough <strong>for</strong> aluminum as well as silicon to be<br />
oxidized 8 . Precipitation is preferred at grain boundaries<br />
which are short diffusion pathways <strong>for</strong> oxygen. It is<br />
believed that the alumina veins may act as preferential sites<br />
<strong>for</strong> crack initiation. Once initiated the cracks will open,<br />
exposing new metal surfaces to the gas phase and oxidation<br />
<strong>of</strong> the crack edge would occur with growth <strong>of</strong> a chromiumrich<br />
oxide. Eventually, the chromium oxide may fully fill<br />
the crack, <strong>for</strong>ming a large region filled with chromium<br />
oxide.<br />
Following an equivalent process, <strong>for</strong>mation <strong>of</strong><br />
intergranular alumina was observed at grain boundaries<br />
intersecting with main oxidized cracks, including ahead <strong>of</strong><br />
the crack tip, as shown in Figure 7b. Cracks are likely to<br />
propagate preferentially through these brittle alumina<br />
precipitates and the crack growth may be accelerated.<br />
There<strong>for</strong>e, internal oxidation <strong>of</strong> alumina first below the<br />
external chromia scale and then ahead <strong>of</strong> the crack tip may<br />
increase both crack initiation and propagation rate. This<br />
hypothesis is consistent with the observed intergranular<br />
cracking and may account <strong>for</strong> at least a portion <strong>of</strong> the<br />
reduction in the <strong>fatigue</strong> life with a tensile hold<br />
IV. CONCLUSIONS<br />
This paper reviews two previous publications by<br />
Carroll and co-workers 10,11 on creep-<strong>fatigue</strong> testing <strong>of</strong> Alloy<br />
617 in air and in a <strong>VHTR</strong> simulated impure helium at<br />
950°C at total strain ranges <strong>of</strong> 0.3% and 0.6%. This work<br />
supports acceptation <strong>of</strong> Alloy 617 in the nuclear section<br />
(section III) <strong>of</strong> the ASME code <strong>for</strong> application at high<br />
temperature as well as licensing <strong>of</strong> <strong>VHTR</strong> systems with<br />
IHX. The creep-<strong>fatigue</strong> behavior <strong>of</strong> Alloy 617 at 950°C<br />
may be influenced by both the environment and the creep<br />
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Paper 11284<br />
de<strong>for</strong>mation that occurs during the tensile hold. The shift in<br />
crack initiation mode from transgranular during <strong>fatigue</strong><br />
de<strong>for</strong>mation to intergranular during creep-<strong>fatigue</strong><br />
de<strong>for</strong>mation likely results from the environmental<br />
influence. Oxidation may also play a role in determining<br />
the crack propagation mode, tending the creep-<strong>fatigue</strong><br />
crack propagation to intergranular as opposed to<br />
transgranular. However, longer hold times did not result in<br />
the further decrease in cycle life suggesting that the<br />
environmental influence on creep-<strong>fatigue</strong> crack propagation<br />
is not the controlling factor. Measurements <strong>of</strong> the oxidation<br />
phenomena are planned <strong>for</strong> a more quantitative approach.<br />
Constant accumulated creep damage despite an increasing<br />
hold time agrees well with the experimental tendency <strong>of</strong><br />
cycles to failure saturating. The creep damage in the alloy<br />
bulk, in the <strong>for</strong>m <strong>of</strong> grain boundary cracking, may have<br />
accelerated the crack propagation. The amount <strong>of</strong> grain<br />
boundary cracking was similar among all <strong>of</strong> the hold times<br />
due to the rapid saturation during the stress relaxation.<br />
<strong>Creep</strong>-<strong>fatigue</strong> testing will be per<strong>for</strong>med under another<br />
helium environment producing different microstructure and<br />
corrosion products to determine any change in the<br />
de<strong>for</strong>mation mechanisms.<br />
ACKNOWLEDGMENTS<br />
The authors would like to acknowledge Joel Simpson,<br />
DC Haggard, Dave Swank, Randy Lloyd, Tammy<br />
Trowbridge, Todd Morris and Barry Rabin <strong>for</strong> conducting<br />
the experiments and the microscopy. This work was<br />
supported through the U.S. Department <strong>of</strong> Energy Nuclear<br />
Energy.<br />
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