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Materials Science and Engineering A 518 (2009) 65–75

Contents lists available at ScienceDirect

Materials Science and Engineering A


journal homepage: www.elsevier.com/locate/msea

Application of the Monkman–Grant law to the creep fracture of


nodular cast irons with various matrix compositions and structures
E. Hug a,∗ , C. Keller a , J. Favergeon b , K. Dawi b
a
Laboratoire de Cristallographie et Sciences des Matériaux, ENSICAEN, Université de Caen, CNRS, 6 Bd Maréchal Juin, 14050 Caen, France
b
Laboratoire Roberval, UMR6253 CNRS, Centre de Recherches de Royallieu, Université de Technologie de Compiègne, BP 20529, 60205 Compiègne, France

a r t i c l e i n f o a b s t r a c t

Article history: Creep behaviour of nodular cast irons with three different matrix compositions and microstructures has
Received 20 January 2009 been investigated up to fracture in the elastic regime for temperatures between 650 ◦ C and 900 ◦ C. The
Received in revised form 7 April 2009 elastic stress levels were chosen taking into account the non-linear dependence between elastic stresses
Accepted 9 April 2009
and corresponding strains. Results show that austenitic cast irons are more creep resistant than ferritic
ones. However, all materials obey to a single Monkman–Grant law. Fracture of samples with short life
Keywords:
times is dominated by the plastic straining of the matrix independently of their metallurgical state. Creep
Creep tests
fracture of long life time samples is controlled by diffusion mechanisms like cavity nucleation on the
Nodular cast irons
High temperature deformation
grain boundaries. It is shown that the damage growth in secondary and tertiary creep regimes can be
Fracture represented by a single parameter whatever the creep mechanisms and the metallurgical properties of
Creep damage nodular cast irons.
© 2009 Elsevier B.V. All rights reserved.

1. Introduction [8]. The evaluation of the damage with mechanical loading was
successfully studied using electric resistance measurements [9],
Nodular cast irons (NCI) are widely used in the automotive ultrasonic non-destructive tests [10] or evolution of the Young
industry because of the relative low cost fabrication of products modulus with plastic strain [7]. Nevertheless, all these works deal
with complicated shapes. These materials exhibit good mechanical with mechanical behaviour at room temperature. High temper-
properties, especially for the use in cyclically loaded components ature properties were partly studied by Lesueur et al. [11] for
[1–3]. Some automotive components, like manifolds, must be ultrahigh-carbon steels, containing typically 1–1.8 wt.%C, but their
dimensionally stable at high temperature, typically around 800 ◦ C. work focused on creep response at strain rates and temperatures
These structural components are subjected to relatively low and characteristic of hot metal forming. Kosinskii [12] has analyzed the
constant stresses in the elastic regime, which can produce creep effect of secondary elements as Cr or Ti on the creep behaviour of
straining, damage, and occasionally fracture. Ferritic SiMo based cast iron. Lui and Chao [13] have shown that brittleness can appear
NCI are currently employed with various alloy elements for the con- at moderately high temperatures in ferritic NCI (typically less than
ception of manifolds. These alloys give a good compromise between 500 ◦ C). This effect can be attributed to dynamic strain ageing and
economical considerations, mechanical properties and high tem- triaxial stress field developed in the ferritic matrix. Other mechan-
perature corrosion resistance. Nevertheless, for higher exhaust gas ical studies are then necessary to understand the creep behaviour
temperatures, austenitic Ni-rich NCI are often preferred in order to of NCI at higher temperatures.
enhance the mechanical properties and prevent decarburization as The main goal of this work is to give experimental results con-
well as phase transformation. cerning the creep behaviour of three NCI submitted to stresses in the
Damage and fracture of NCI can be classically attributed to elastic regime for temperatures ranging between 650 ◦ C and 900 ◦ C.
nucleation, growth and coalescence of voids at the graphite/matrix Monotonous tensile tests were firstly carried out at various temper-
interface [4]. Various studies were devoted to this topic, for atures to evaluate the yield stress taking into account the non-linear
monotonous tensile stress conditions [5], cycling loading [6] or frac- dependence between stress and strain in the elastic regime, follow-
ture toughness [7]. In general, strengthening and ductility of cast ing previous work of Kohout [14] extended to high temperatures.
irons decrease as the proportion of non-nodular graphite increases Creep tests were then performed up to fracture for various tem-
perature/stress conditions and a single Monkman–Grant law was
established for the three alloys. The mechanisms of creep damage
∗ Corresponding author. Tel.: +33 2 31 45 13 13; fax: +33 2 31 95 16 00.
and fracture were analyzed using microstructural observations and
E-mail address: eric.hug@ensicaen.fr (E. Hug).
quantitative measurements of the primary graphite dimensions.

0921-5093/$ – see front matter © 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2009.04.020
66 E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75

Table 1
Chemical composition of the three nodular cast irons A, B and C.

Composition (wt.%)

C Si Ni Mo Cr Mn Mg P Fe

A 3.2 3.9 0.03 0.54 0.03 0.12 0.03 0.03 Balance


B 2.85 4.6 0.03 0.7 0.8 0.3 0.07 0.04 Balance
C 1.8 5.2 35.3 0.008 2.0 0.3 0.07 0.02 Balance

This approach is closely related to previous works of Eggeler and observed, together with spheroidized pearlite and Mo-rich car-
co-workers [15,16] which used mechanistically based parameters bides.
to quantify cavitation creep damage for the purpose of life assess- The second family of NCI, labelled B, is a ferritic cast iron with
ment of high temperature components. Finally, damage evolution in higher chromium content than the A type (0.8 against 0.03 in wt.%).
NCI under creep conditions was evaluated using a damage param- The corresponding microstructure consists of primary graphite and
eter linking the strain rate at a given time to the minimum strain ferritic grains surrounded by large areas of (Mo, Cr, Mn) rich car-
rate. bides (Fig. 1(b)) depicted by EDS analysis.
The third family, labelled C, is an austenitic nodular cast iron
2. Metallurgical properties of the nodular cast irons of grade D-5S according to ASTM A439 standard. The austenitic
phase is obtained thanks to a high nickel content (>35 wt.%). Pri-
Three families of NCI were studied. Nominal compositions were mary graphite is revealed by microstructural analysis (Fig. 1(c)).
given by the foundry and partly confirmed by EDS and WDS mea- High chromium content involves the existence of large areas of
surements (Table 1). Microstructural features were studied using chromium rich carbides.
light microscopy and scanning electron microscopy (SEM). The Thermo-Calc software (TTNF5 database) was used to obtain
The first type of cast iron, labelled A, is a classical ferritic SiMo the Fe-C phase diagram of each NCI (Fig. 2). Materials are very close
NCI, with roughly 5% of pearlite. This alloy is optimized for ther- to the eutectic composition, each of them being hypoeutectic. These
momechanical applications in automotive industry. Fig. 1(a) shows calculations show that the A and B cast irons exhibit a ferritic matrix
the microstructure of this material: primary graphite is clearly from room temperature to roughly 850 ◦ C. In consequence, the max-

Fig. 1. Microstructure of the three studied NCI obtained by light microscopy and SEM. Ferritic SiMo grade A (a), ferritic rich chromium grade B (b), and austenitic nickel and
chromium rich grade C (c).
E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75 67

Fig. 2. Sections of the NCI Fe-C phase diagram computed by Thermo-Calc. NCI A with 3.9 wt.%Si, 0.54 wt.%Mo, 0.12 wt.%Mn (a); NCI B with 4.6 wt.%Si, 0.7 wt.%Mo, 0.8 wt.%Cr,
0.3 wt.%Mn (b); NCI C with 5.2 wt.%Si, 35.3 wt.%Ni, 2 wt.%Cr, 0.3 wt.%Mn (c).

imum creep temperature for NCI A and B was restricted to 800 ◦ C M corresponding to (Fe, Ni, Cr, Si), and at low temperature, the cast
in order to avoid the ␣ ↔ ␥ transformation. The other interesting iron exhibits M7 C3 carbides with M corresponding to (Fe, Mn, Ni,
point concerns the nature of the carbides which are mainly of the Cr). The maximum creep temperature has been fixed to 900 ◦ C for
M6 C type. M7 C3 carbides appear only at low temperature (below NCI C.
250 ◦ C). The M6 C carbides exhibit a chemical formula given as (Fe, Metallurgical properties of the various NCI are summarized
Mo, Cr, Si)6 C, and the M7 C3 carbides are of the type (Fe, Mo, Mn, in Table 2. Mean grain size and crystallographic texture were
Cr)7 C3 . The EDS analyses are actually not sufficient to discriminate computed by conventional metallography and using EBSD on elec-
these different carbides. tropolished samples. Nodule parameters (i.e. their volume fraction
For the C type cast iron, the austenitic matrix remains stable at fvol , their mean radius rN and their sphericity S) were obtained
low temperature. From the phase diagram, a ␥ phase appears below thanks to numerical treatment of surface images of polished and
580 ◦ C which corresponds actually to a modified austenite whose etched samples. S = 1 for an ideal spheroidal form of graphite.
composition differs a little compared to the primary ␥ austenite. For the three NCI, the mean grain size ranges between 23 ␮m
Some ferrite also appears below 500 ◦ C on the phase diagram. Actu- and 42 ␮m with a typical standard deviation around half the grain
ally, this phase is not observed experimentally. For this austenitic size. Austenitic NCI exhibits the smallest grain size and the smallest
cast iron, the high temperature carbides are of the M6 C type with volume fraction of the carbon nodules (8.6% against 11.1% and 10.1%
68 E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75

Fig. 3. Normalized {1 1 1}, {0 0 1} and {0 1 1} inverse pole figures for ferritic A and B (a) and austenitic C (b) NCI (EBSD measurements, CD: creep direction, RD: radial direction).

for NCI A and B, respectively). The sphericity of the nodules is very samples with 6 mm diameter and 25 mm gauge length. The test
similar for all NCI, ranging between 96% and 99%. All alloys exhibit was strain rate controlled at a strain rate of 6.67 × 10−4 s−1 . Axial
weak crystallographic textures with a maximal density lower than deformation was measured by a classical high temperature contact
5 m.r.d. (Fig. 3). Moreover, the same dominant pole 0 0 1 lies paral- extensometer.
lel to the creep direction. Consequently, the mechanical behaviour Cylindrical creep test samples having a diameter of 7.5 mm and a
of the three NCI will be supposed not to be affected by their crys- gauge length of 25 mm were machined directly from ingots. Forty-
tallographic texture. three tensile creep tests were carried out on the three families
of NCI using constant-load machines. Creep strain was monitored
3. Thermomechanical behaviour of NCI using two parallel extensometers incorporating a linear variable
displacement transducer. The knife edges of the extensometers
3.1. Experimental methods were clamped to the specimen grips. Creep strains were measured
with a precision of 10−4 . Five temperatures were used for the exper-
The non-linear dependence between stress and strain in the iments: 650 ◦ C, 700 ◦ C, 750 ◦ C, 800 ◦ C and 900 ◦ C (the latter value
elastic regime was first investigated. To this end, uniaxial tensile concerning only NCI C, as explained above).
tests were performed at various temperatures between room tem-
perature and 900 ◦ C on axisymmetric cylindrical dog bone shape 3.2. Tensile behaviour

Tensile behaviour of NCI A (ferritic) and C (austenitic) are given


Table 2
in Fig. 4(a) and (b) at room temperature and at 800 ◦ C, respectively.
Metallurgical characterization of the metallic matrix and the graphite nodules of the
three NCI (d: mean grain size, I: intensity of the crystallographic texture, fvol : volume Evolutions of conventional yield stress  e0.2 (measured for a plastic
fraction of the nodules, rN : mean radius of graphitic nodules and S: sphericity). strain of 0.2%) and ultimate tensile stress  u with temperature are
shown in Fig. 4(c).
Metallic matrix Nodules
For temperatures between 650 ◦ C and 900 ◦ C, the austenitic NCI
Nature d (␮m) I (m.r.d.) fvol (%) rN (␮m) S exhibits better properties than the ferritic one: higher strain hard-
A Ferritic 35 1.96 11.1 8 0.96 ening, higher values of  e0.2 and  u . The viscoplastic behaviour of
B Ferritic 42 1.73 10.1 11 0.97 NCI A at these temperatures is creep like: the plastic yielding occurs
C Austenitic 23 4.90 8.6 9 0.99
for a constant stress value, very close to the yield stress. The same
E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75 69

phenomenon is observed for NCI C but the creep like behaviour


appears for temperatures higher than 750 ◦ C. NCI of type B, which
contains (Mo, Cr, Mn) rich carbides, displays mechanical properties
very similar to the conventional ferritic one (type A).
Kohout [14] has previously outlined the strong non-linear
dependence between stress and strain in the elastic regime of nodu-
lar cast irons. The deviation from the classical Hooke’s law can
be correlated with the graphite shape and the metallurgy of the
matrix. This effect was observed in all tensile tests performed in
this study. Moreover, this phenomenon is clearly enhanced with an
increase in temperature. The following relationship between the
stress  and the strain ε in the elastic regime can successfully be
used [14]:
E0 ε
= . (1)
1 + ε
E0 is the initial elastic modulus, taken as the slope at the origin of the
stress–strain curve.  is the parameter representing the deviation
from Hooke’s law (non-linearity coefficient). Fig. 5(a) shows the
very beginning of the stress–strain curve of ferritic NCI resulting
from a tensile test at 800 ◦ C. In this graph are also indicated the
initial elastic modulus and the way to compute the non-linearity

Fig. 4. Monotonous tensile behaviour with temperature of ferritic (A) and austenitic
(C) NCI. Tensile stress–strain curves at (a) room temperature and (b) 800 ◦ C. Evo-
lution of the conventional yield stress  e0.2 and ultimate tensile stress  u with
Fig. 5. Stress–strain curve of NCI A (800 ◦ C) for strains up to 0.5%: definition of the
temperature (c).
initial elastic modulus E0 and the deviation parameter  (a). Evolution of  with
temperature for the three NCI (b).
70 E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75

coefficient. The intersection between the stress–strain curve and a


secant of slope E0 /2 directly gives an abscissa of 1/.
The evolution of  with the temperature is given in Fig. 5(b) for
each NCI. All materials have roughly the same value of  at room
temperature, typically around 150. Ferritic alloys then show a much
stronger non-linearity for higher temperatures than the austenitic
one.
As a result, the conventional yield stress  e0.2 is not a perti-
nent parameter giving the transition between the elastic and the
viscoplastic regime. In order to guarantee that creep tests are car-
ried out in the elastic regime, the values of the creep stresses were
chosen taking into account the non-linearity coefficient given in
Fig. 5(b).
Thanks to Eq. (1), the corrected elastic limit  ecor is therefore
computed using the following relationship:
e0.2 (T )
ecor (T ) = . (2)
1 + 0.002(T )
Conventional yield stresses  e0.2 and corrected values  ecor are
given in Table 3 for each NCI and for the temperatures of the fol-
lowing creep tests.  ecor values appear to be much lower than
conventional yield stresses in all cases.

3.3. Monkman–Grant law

For the temperatures given in Table 3, creep tests were carried


out at various stresses, taking into account the values of  ecor . These
different tests lead to fracture times ranging from 2 h to 4000 h.
Fig. 6 shows creep curves and corresponding creep rates
obtained at 800 ◦ C with various applied stresses for ferritic and
austenitic NCI. Creep results for 20 MPa of applied stress and various
temperatures are presented in Fig. 7. Creep curves are normalized
using the fracture parameters trupt and εrupt which are the lifetime
and the corresponding fracture strain, respectively [17].
After a very short primary creep domain, the specimens exhibit
a more or less pronounced second stage with a minimum creep rate
value ε̇min , followed by a long tertiary period which corresponds to
the progressive damage of the sample up to the fracture. Plotting
the strain rate evolution versus the strain shows that ε̇min really
represents a local minimum rather than a steady-state domain, in
accordance with previous works [18–20]. Depending on the values
of the applied stress, the minimum creep rate is reached at a time
which is roughly equal to [0.01–0.3]trupt . Next the tertiary creep
Fig. 6. Normalized creep curves (a) and corresponding creep rate curves (b) for
stage progressively becomes the dominant feature of the creep 800 ◦ C.
behaviour.
The minimum creep rate ε̇min can be classically linked to the
fracture time trupt using the Monkman–Grant (MG) relationship thickness on long time creep test samples: the oxide thickness
[21,22]: does not exceed a few percent of the total diameter of the sam-
ples. Moreover, Fig. 2 shows that the austenitic phase appears for
ε̇m t rupt = k (3)
min
temperature above roughly 850 ◦ C for ferritic NCI A and B. This
where k and m are the MG constants. The exponent m is typically value was also determined experimentally by differential scanning
close to unity when creep fracture is entirely controlled by creep calorimetry (DSC) and equals to 870 ◦ C. The maximum creep tem-
strain [18]. A double-logarithmic representation of this relationship perature used in this study for ferritic alloys is 800 ◦ C. So, one can
applied to the experimental results is shown in Fig. 8. It is note- assume that the metallic matrix remains ferritic during creep tests.
worthy that all the experimental results can be fitted with a very For NCI of type C, the matrix remains austenitic whatever the test
good confidence by a single set of parameters: k = 0.15 ± 0.06 and temperature, so no phase transformation of the matrix occurs in
m = 0.91 ± 0.04. the experiments. Therefore, the main metallurgical modification
of the material during long time creep experiments concerns the
4. Discussion evolution of the carbides.
The uniqueness of the MG law for the various NCI suggests that
Various metallurgical aspects can influence the creep behaviour similar damage mechanisms take place in these alloys. In order to
of NCI, especially for long time tests and high temperature levels. clarify this point, microstructural observations were carried out on
Among them we can cite high temperature oxidation [23,24] or two fractured samples of each family of NCI. Samples were cho-
metallurgical transformations. We suppose in the following that sen with short (typically 15 h) and long (typically 950 h) fracture
fracture tests are not fundamentally influenced by specimen oxida- times. A damage parameter  was computed and its variation was
tion. This hypothesis is reinforced by measurements of the oxide evaluated as a function of the relative lifetime t/trupt .
E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75 71

Table 3
Conventional yield stresses ( e0.2 ) and corrected corresponding values ( ecor ) taking into account the deviation of the Hooke’s law. Results are given for the three NCI tested
and for the different creep temperatures (all values in MPa).

650 ◦ C 700 ◦ C 750 ◦ C 800 ◦ C 900 ◦ C

 e0.2  ecor  e0.2  ecor  e0.2  ecor  e0.2  ecor  e0.2  ecor

NCI A 122 46 92 31 52 16 37 11
NCI B 127 51 85 31 49 16 39 11
NCI C 165 105 142 90 135 85 100 59 52 29

4.1. Microstructural features

Figs. 9–11 show typical microstructures of the materials frac-


tured by creep after short and long time experiments.
Short time fractured specimens have / ecor values typically
higher than 0.7. Ferritic NCI exhibit strong plastic straining of the
ferritic grains (Fig. 9(a) for NCI A, Fig. 10(a) for NCI B). Consid-
erable stretching of carbon nodules and nodule-bearing cavities
are also depicted, as shown in the insert of Fig. 9(a). Small voids
are also present at the interface between graphite and matrix.

Fig. 8. Monkman–Grant graph for the three NCI.

Austenitic NCI shows the same microstructural evolution as ferritic


ones, except that the nodules stay grossly spherical after deforma-
tion (Fig. 11(a)). Microfissuration appears in the area of carbides
oriented perpendicularly to the stress direction (Fig. 11(a), right
picture).
The evolution of the sphericity of the nodules was computed
using image analysis carried out on short time fractured samples.
This parameter was evaluated in planes containing the direction of
the creep stress (SL ) and in transverse sections to the creep stress
(ST ). Results are given in Table 4.
These measurements clearly indicate a strong elongation of the
nodules along the stress direction, due to plastic straining. The exis-
tence of voids at the interface between the metallic matrix and the
graphite nodules explains the relatively lower value of ST after creep
straining.
The creep fracture of NCI is therefore controlled by the plastic
straining for the higher minimum creep rate values (i.e. the shorter
fracture times). These mechanisms are similar to those occurring
in tensile tests at high temperatures (“creep like” behaviour).
For long time fractured samples, / ecor values are typically
lower than 0.4. No deformation of the grains is observed in this
case, whatever the nature of the matrix (ferritic or austenitic).
This observation goes with a partial dissolution of the carbides
in the matrix. Moreover, the void volume fraction between the
graphite and the matrix is important, especially for ferritic materi-
als (Fig. 9(b)). The diameter of graphitic nodules decreases but their
sphericity remains roughly unchanged. The fracture of the samples
is intergranular in nature, microcracks being nucleated close to the
Fig. 7. Normalized creep curves (a) and corresponding creep rate curves (b) for a
primary graphite along the grain boundaries or along the remain-
stress of 20 MPa. ing carbides (Fig. 10(b)). The coalescence of these cavities leads to
72 E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75

Fig. 9. Microstructure of NCI A fractured by creep. Short time, trupt = 13.6 h, 750 ◦ C, / ecor = 0.81 (a). Long time, trupt = 995.6 h, 800 ◦ C, / ecor = 0.34 (b). Arrows indicate the
stress direction.

intergranular crack propagation easily observable in areas close to (T, ) compared with ferritic NCI. Nevertheless, when this value is
the fracture surface (Figs. 9(b), 10(b) and 11(b)). Large cracks have reached, the rupture lifetime is the same for all the NCI. The damage
formed perpendicular to the stress axis, in a similar way than pre- in secondary and tertiary creep could therefore be represented by
viously observed in 12% Cr–Mo–V steels crept at low stress levels a single parameter whose value allows the comparison of the creep
[15]. resistance of the various NCI.
The creep fracture of NCI is then controlled by the cavity nucle- Using an approach proposed by Riedel [25,26], the strain rate ε̇
ation and its diffusive growth for the lower minimum creep rate can be linked to the minimum strain rate ε̇min thanks to a damage
values (i.e. the longer fracture times) whatever the nature of the parameter :
metallic matrix.
ε̇min
ε̇ = (4)
1−
4.2. Evaluation of the damage during creep test
The evolution of the damage parameter with the creep strain ε
Microstructural observations show that the mechanisms can be written as:
responsible for the plastic straining (short fracture times) and for  ε ˛
the cavity nucleation and growth (long fracture times) are the same = , (5)
εrupt
for all the NCI, in agreement with the single MG law. Austenitic NCI
are more creep resistant than ferritic ones: a given value of the min- where ˛ is an adjustable parameter. Integrating Eq. (4) with the
imum creep rate is obtained for higher values of the parameters help of Eq. (5) gives a relationship describing the creep curve in
E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75 73

Fig. 10. Microstructure of NCI B fractured by creep. Short time, trupt = 17.4 h, 750 ◦ C, / ecor = 0.94 (a). Long time, trupt = 966.7 h, 800 ◦ C, / ecor = 0.36 (b). Arrows indicate the
stress direction.

secondary and tertiary stages: , is the creep damage tolerance previously introduced by Ashby

εrupt
 ε ˛+1 and Dyson [27]. The combination of Eqs. (5)–(7) leads to the fol-
ε̇min t = ε − . (6) lowing relation between the lifetime and the damage parameter:
˛+1 εrupt
t
The creep fracture is obtained when t = trupt and ε = εrupt . Eq. (6) = −1 − ( − 1) . (8)
t rupt
gives for this particular case a relation between the parameter ˛
and the creep parameters:  has been computed for the six creep fracture tests whose
microstructures are shown in Figs. 9–11 (Table 5). Corresponding
εrupt ˛+1 εrupt damage curves have then been plotted in Fig. 12.
ε̇min trupt = εrupt − ⇒ == . (7)
˛+1 ˛ ε̇min t rupt For long lifetime creep tests, controlled by the nucleation
and growth of cavitating boundary facets, the damage parameter
strongly rises in the first 10% of the lifetime, and then increases
Table 4
Sphericity values in planes containing the stress direction (SL ) and in transverse
sections (ST ) for the three families of NCI in the initial state and after creep fracture
Table 5
for a time around 15 h.
Values of the creep damage parameter  for the six fractured tests observed in
Initial state Creep fractured samples, trupt ≈ 15 h Figs. 9–11.

SL = ST SL ST Short lifetime (trupt ≈ 15 h) Long lifetime (trupt ≈ 950 h)

NCI A 0.96 0.64 0.92 NCI A 2.3 6.2


NCI B 0.97 0.75 0.95 NCI B 2.1 9.2
NCI C 0.99 0.92 0.96 NCI C 1.9 4.9
74 E. Hug et al. / Materials Science and Engineering A 518 (2009) 65–75

more slowly and monotonously up to fracture. This behaviour is


similar to the variation of  with t/trupt computed by Eggeler [16]
for a (2.25 wt.%Cr, 1 wt.%Mo) steel. This result can be correlated with
an early cavity nucleation for the three NCI, when dominant creep
mechanism is diffusion. Moreover, this nucleation could occur con-
tinuously during creep [15]. Austenitic alloy is less sensitive to
cavity nucleation. This result can be related to the self-diffusion
activation energy of iron in ␥-Fe (310 kJ/mol) smaller than the one
in ␣-Fe (280 kJ/mol) [28]. Ferritic alloy with high chromium content
is strongly subject to damage in the earlier time of creep solicita-
tions in the diffusive regime. (Mo, Cr, Mn) rich carbides present in
great proportion in NCI B could act as preferential sites for cavity
nucleation.
Short lifetime creep tests are controlled by plastic straining of
the metallic matrix and plastic straining of the nodules for fer-
ritic alloys.  monotonously increases with time test whatever the
alloy. The value of the creep damage tolerance  is relatively low
in this case. This could be related to transgranular fracture modes
[29] when plasticity of the matrix is the governing process. The
 parameter could be associated in this regime to the incompat-
ibilities of strains occurring between the metallic matrix and the
graphite nodules.

5. Conclusions

The creep fracture properties of various NCI were investi-


gated at temperatures between 650 ◦ C and 900 ◦ C, for elastic
applied stresses. These alloys differ by their metallurgical (carbides,
grain sizes, nodular parameters) and crystallographic (ferritic or
austenitic matrix, textures) properties. The stresses were chosen to
be in the elastic range taking into account the strong non-linearity
of Hooke’s law observed in these materials, especially at higher
temperatures. The relation between the minimum creep rate and
the fracture time obeys a Monkman–Grant law which implies sim-
Fig. 11. Microstructure of NCI C fractured by creep. Short time, trupt = 16.4 h, 800 ◦ C, ilar creep mechanisms for the three tested NCI.
/ ecor = 0.78 (a). Long time trupt = 904.5 h, 900 ◦ C, / ecor = 0.35 (b). Arrows indicate Microstructural observations of the fractured samples lead to
the stress direction. the following conclusions:

• Low lifetime samples exhibit strong plastic straining of the


metallic matrix. Strong straining of the nodules also appears in
the ferritic NCI unlike austenitic ones. Microcracks are mainly
observed in the neighbourhood of metallic carbides.
• Long time rupture creep specimens show numerous creep cavi-
tations which tend to agglomerate to form microcracks and voids
at the interfaces between matrix and nodular graphite. No defor-
mation of the ferritic or austenitic grains is observed.

Damage therefore occurs in NCI in a similar way for short time


fracture tests (plastic straining) and for long time creep experiments
(cavity nucleation). This can be highlighted by the use of a single
damage parameter following a formalism proposed by Riedel and
using the creep damage tolerance introduced by Ashby and Dyson.
Concerning the potential use of NCI in structural components
as manifolds, for higher temperatures than today, it is critical to
enhance the mechanical resistance of the interfaces in order to pre-
vent cavitation. One way could be to elaborate dual microstructure
around nodular graphites to make the initiation of cracks between
graphite and matrix more difficult, as already pointed out in previ-
ous studies [5,30].

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