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Materials Science and Engineering A 387–389 (2004) 599–603

Effect of the microstructure on the creep behavior of PM Udimet 720


superalloy—experiments and modeling
Sophie Dubiez-Le Goff, Raphaël Couturier∗ , Laure Guétaz, Hélène Burlet
CEA-Grenoble, DTEN/SMP/LS2M, 38054 Grenoble Cedex 9, France

Received 25 August 2003; received in revised form 22 January 2004

Abstract

Powder metallurgy processed Udimet 720 is a high creep strength nickel-based superalloy considered for high temperature turbine
disks for nuclear gas cooled reactors working under 700 ◦ C. Both fine-grained and coarse-grained microstructures have been obtained by
applying respectively a subsolvus or a supersolvus solution treatments, followed by ageing treatments. In both microstructures, the distri-
bution of the strengthening ␥ precipitates has been characterized by transmission electron microscopy (TEM). The creep curves of the
coarse-grained microstructure show the three usual creep stages. On the contrary, the creep curves of the fine-grained microstructure show
a transition directly from primary to apparent tertiary creep without any obvious steady state. According to TEM analyses, Orowan loops
surround Udimet 720 CR ␥ and U720 HS ␥ at high stress whereas U720 HS ␥ are sheared at low stress. To describe the behavior of
the superalloy Udimet 720, a specific creep model is developed on the basis of McLean and Dyson models including physical damage
parameters.
© 2004 Published by Elsevier B.V.

Keywords: Ni-based superalloy; Powder metallurgy; Udimet 720; Creep; TEM; Dislocations

1. Introduction has been developed [2]. It includes the resulting physical


damage parameters previously identified.
Nickel-based superalloys are considered for high tem-
perature gas turbines of nuclear gas cooled reactors (GCR).
The gas turbine disks, with a diameter about 1.5 m, are 2. Material and experimental methods
expected to work at a maximum temperature of 700 ◦ C
during around 60 000 h without significant maintenance. The chemical composition of U720 is given in Table 1.
Powder metallurgy (PM) processing seems appropriate to Powder particles are obtained by atomization under argon
produce segregation-free parts, with a geometry close to the atmosphere. The particle diameter ranges from 10 to 90 ␮m
final shape of the component. Since a material with high with an average diameter of about 30 ␮m. Powder billets
creep strength is required for this application, PM Udimet used in this study have been consolidated using the hot
720 LI (U720) is considered as a potential superalloy [1]. isostatic pressing (HIP) facility of Aubert&Duval-Holding
The creep behavior of U720 was therefore investigated by under 1400 bar at 1100 ◦ C during 3 h.
conducting creep tests at 650 ◦ C on two microstructures ob- Both heat treatments applied are the usual ones for
tained from two different heat treatments. The deformation cast and wrought U720 [3], known as high strength (HS),
and damage mechanisms have been analysed, and a creep improved for tensile strength and low cycle fatigue re-
predictive model based on McLean and Dyson approach sistance, and creep resistant (CR), improved for creep
strength. HS treatment consists of a 4 h solutioning treat-
ment at 1110 ◦ C, followed by two precipitation heat treat-
∗ Corresponding author. Tel.: +33 4 38 78 35 59; ments for 24 h at 650 ◦ C and 16 h at 760 ◦ C. The CR
fax: +33 4 38 78 58 91. heat treatment consists of a 4 h solutioning at 1170 ◦ C,
E-mail address: raphael.couturier@cea.fr (R. Couturier). then a second 4 h solutioning at 1080 ◦ C, followed by two

0921-5093/$ – see front matter © 2004 Published by Elsevier B.V.


doi:10.1016/j.msea.2004.01.094
600 S. Dubiez-Le Goff et al. / Materials Science and Engineering A 387–389 (2004) 599–603

Table 1
Chemical composition (wt.%) of the Udimet 720 LI
Ni Bal.
Cr 16.2
Co 15.3
Ti 5.18
Mo 3.06
Al 2.47
W 1.33
Fe 0.06
Zr 0.039
C 0.023
Cu 0.02
B 0.018
Si 0.007

precipitation heat treatments for 24 h at 845 ◦ C and 16 h at


760 ◦ C.
Creep tensile tests have been performed under air at
650 ◦ C on cylindrical specimens (Ø4 mm) after either HS
or CR heat treatments under stresses ranging from 600 to
900 MPa. Stress range applied to the specimens was se-
lected to reach fracture between 10 and 5000 h. Creep tests
have been conducted under constant load and tensile tests
have been performed at 5 × 10−4 s−1 .
To analyse the dislocation structure by transmission elec-
tron microscopy (TEM) in the strained specimens, thin foils
were machined out from specimens strained up to 1% and
3% by creep and tensile tests.

Fig. 1. ␥ distribution in U720 HS (a) and CR (b)—TEM dark-field


3. Experimental results micrograph using 0 1 1 ␥ diffraction spot.

3.1. Microstructures than the CR one. Moreover, U720 CR shows the usual three
stages of creep whereas U720 HS shows a transition directly
HS and CR heat treatments, mainly differing by their so- from primary to tertiary creep, exhibiting a point of inflection
lutioning temperature, resulted in two microstructures. Sub- corresponding to the minimum creep rate.
solvus solutioning of the U720 HS leads to a ␥-grain size
ranging from 1 to 10 ␮m. Supersolvus solutioning of the
U720 CR leads to ␥-grain size ranging from 10 to 30 ␮m.
In both microstructures, ␥ precipitates constitute about
50% of the volume fraction of the alloy. Fig. 1 shows the
distribution of the ␥ in the two microstructures. For U720
HS, there are three different types of ␥ (Fig. 1a) : primary
␥ formed during HIP treatment, with a diameter of 450 nm,
then secondary and tertiary ␥ nucleated during cooling after
solutioning treatment and coarsened during ageings, with
respective average diameters of 40 and 10 nm. For U720 CR,
only two types of ␥ are formed during cooling (Fig. 1b) :
the secondary ␥ with a diameter of 300 nm and the tertiary
ones with a diameter of 30 nm.

3.2. Creep behavior at 650 ◦ C

Strain versus time curves of 650 ◦ C creep tests performed


on U720 HS and U720 CR show two different behaviors Fig. 2. Creep curves at 650 ◦ C of the Udimet 720 HS and CR under
(Fig. 2): under the same stress, U720 HS creep life is longer stress ranging from 600 to 900 MPa.
S. Dubiez-Le Goff et al. / Materials Science and Engineering A 387–389 (2004) 599–603 601

4.1. Early damage by micro-cracking and cavity


nucleation of the specimen

This hypothesis does not seem relevant at 650 ◦ C, as only


few micro-cracks are observed very close to the fracture sur-
face on longitudinal cross-section of broken specimens. At
750 ◦ C, a lot of cavities and cracks are observed in the bulk of
the specimen after failure. A specific test was therefore con-
ducted to show whether the observed damage is responsible
for the observed softening. A creep test (750 ◦ C/280 MPa)
has been stopped at 2/3 of the creep life. Then, the mi-
crostructure has been restored by applying the full HS heat
treatment cycle to the specimen (under vacuum), and the
creep test was started again until rupture under the same
conditions. The behavior of this rejuvenated specimen looks
like the one of the virgin material. This suggests that the
specimen creep rate is not influenced by cracks or voids af-
ter 2/3 of creep life, when softening is already observed.

4.2. Degradation of the microstructure related to γ  ageing


during creep deformation

Creep softening of superalloy is often related to ageing


as ␥ coarsen during the test. Nevertheless, at 650 ◦ C, TEM
observations have shown that ageing up to 5000 h has no
measurable effect on ␥ precipitate size.

Fig. 3. Dislocation structures in the Udimet 720 HS (a) and Udimet 720 4.3. Increase of the true stress during deformation
CR (b) (TEM weak-beam) in interrupted specimens crept after 1% strain
under 750 MPa at 650 ◦ C. In this study, creep tests were not conducted under con-
stant stress, but under constant load. The applied stress thus
3.3. Dislocation structures after creep and tensile increases as the strain increases and the section decreases.
tests at 650 ◦ C The true stress is defined as σ = σ 0 exp(ε), with initial stress
σ 0 and true strain ε. As proposed by Maldini and Lupinc
TEM analysis of crept specimen strained at 1% under [4], the true strain rate of the creep tests shown in Fig. 2 are
750 MPa show large stacking faults inside the ␥ for U720 plotted in Fig. 4 as a function of true stress. The decrease
HS (Fig. 3a) and dislocation loops around the ␥ for the U720 of the strain rate corresponds to the primary stage, then the
CR (Fig. 3b). This suggests that the deformation mechanisms increase of the strain rate corresponds to the secondary and
differ from one microstructure to the other: U720 HS ␥ are tertiary stages. On this representation, creep rate was drawn
sheared whereas U720 CR ␥ are bypassed by an Orowan using Norton stress dependence law, as ε̇ ∝ σ n , with Nor-
mechanism. ton coefficient n adjusted to the experimental steady-state or
Crept specimen of U720 HS strained at 3% under 750 MPa minimum creep rate. For U720 CR, n is 20 for the applied
shows even more stacking faults than after 1% strain. By stress range. But a single n-value cannot describe U720 HS
contrast, for U720 HS specimen prestrained at 3% in tensile, stress dependence at all stresses. Thus, for 850 and 900 MPa,
dislocations form loops around the ␥ . n is 24 and for 600, 750 and 800 MPa, n is 12. The plot
of Fig. 4 enables to emphasize the two different kinds of
creep behavior. For U720 CR, after primary stage, curves
4. Discussion fall on the Norton’s law plot. This means that the increase
of the strain rate observed in Fig. 2 corresponds in fact to a
To understand why the creep rate quickly increases after steady-state stage, and that acceleration of creep is only due
the minimum creep rate for HS microstructure, four dif- to the increase of the true stress. U720 HS behavior differs
ferent hypotheses of softening mechanisms are hereafter from high stresses to low stresses. At 850 and 900 MPa, the
investigated: early damage of the specimen, degradation of apparent tertiary stage is linked to the stress increase during
the microstructure related to ageing, increase of the true the creep test, as observed for U720 CR. In contrast at 600,
stress during creep deformation and interaction between 750 and 800 MPa, strain rate increases more quickly than
dislocations and ␥ . Norton’s law prediction. For this stress range, an additional
602 S. Dubiez-Le Goff et al. / Materials Science and Engineering A 387–389 (2004) 599–603

crossing of other dislocations in the same glide plane. In


addition, a higher stacking fault density is observed in the
3% crept U720 HS than in the 1% crept, indicating that there
is no localization of the deformation.
McLean and Dyson proposed an increase of the mobile
dislocation density to explain the softening [2].

5. Modeling

McLean and Dyson proposed a specific model to pre-


dict creep behavior of complex alloy: a physically based
continuum creep damage model with internal state vari-
ables which relates the strain rate response to the applied
stress [2]. The equation of the chosen model results in a set
of a hardening parameter H to describe the primary creep
stage and a parameter Dd to describe the multiplication of
the mobile dislocation density, only for U720 HS at low
stress:
Fig. 4. True strain rate as a function of the true stress for 650 ◦ C creep
 
tests. The rates obtained from Norton law is also drawn as dashed lines. ε̇0 σ(1 − H)
ε̇ = sinh (1)
1 − Dd σ0
damage parameter is required to describe the softening of  
the alloy during creep. h H
Ḣ = 1 − ∗ ε̇, Ḋd = C(1 − Dd )2 ε̇ (2)
σ H
4.4. Dislocation/γ  interactions

TEM analyses indicate that the difference of behavior at


750 MPa is related to different deformation mechanisms:
U720 CR ␥ are by-passed by an Orowan mechanism
whereas U720 HS ␥ are sheared. These two mechanisms,
already observed in other recent PM nickel-based super-
alloys [5,6], seem to be strongly related to the presence
of tertiary ␥ . The large ␥ corridors observed in U720 CR
promote an Orowan mechanism whereas the presence of
tertiary ␥ in U720 HS decreases the corridor width and
promotes a shearing mechanism. According to the previ-
ous investigation, Orowan mechanism observed in U720
CR could be connected to a classical behavior with a
steady state stage, whereas shearing observed in U720 HS
could be connected to a softening mechanism. However,
stress-assisted tertiary stage also appears at high stress for
U720 HS and could thus be related to Orowan mechanism
as for U720 CR. This is confirmed by TEM observations
of interrupted tensile U720 HS specimen showing Orowan
loops around ␥ . The deformation mechanisms hence de-
pend on the stress level. The transition between the two
mechanisms should be the Orowan stress.

4.5. Possible origins of the softening observed at low


strain rate

Particle shearing during deformation is usually associated


with softening of alloys, because particle size decreases in
the glide plane. However, shearing in superalloys implies Fig. 5. Comparison of the model predictions with experimental data of
complex stacking faults [7] which may not facilitate the U720 HS and CR.
S. Dubiez-Le Goff et al. / Materials Science and Engineering A 387–389 (2004) 599–603 603

Table 2 6. Conclusions
Model parameter set for U720 HS and CR used to generate the curves
in Fig. 5
Creep behavior of PM U720 depends on its microstruc-
ε̇0 (s−1 ) σ 0 (MPa) h (MPa) H∗ C ture and stress range. U720 CR and U720 HS crept at high
CR 1.7 × 10−13 34.0 58835 0.08 0 stress are deformed by an Orowan mechanism and present a
HS 1.8 × 10−13 33.7 58357 0.1 1600 steady state stage. By contrast, U720 HS behavior presents
a tertiary stage at low stress that can be related to a ␥ shear-
ing mechanism. These behaviors can be fairly well predicted
by McLean and Dyson creep model by selected physically
based parameters.
with characteristic rate ε̇0 , true stress σ, kinematic back
stress σ 0 , normalized saturation stress H∗ , effective Young
modulus h , and a material constant C. Best parameter sets
References
identified are given in Table 2.
For U720 CR and U720 HS creep at high stress, both
[1] R. Couturier, C. Escaravage, in: Proceedings of the IAEA Technical
having a classical behavior, no damage parameter is required Committee Meeting, IAEA, Palo Alto, CA, 2000.
to describe the full creep curve. For U720 HS at low stress, [2] M. McLean, B.F. Dyson, Eng. Mater. Technol. 122 (2000) 273–278.
softening is modeled by an increase of mobile dislocation [3] M.P. Jackson, R.C. Reed, Mater. Sci. Eng. A 259 (1999) 85–97.
density. [4] M. Maldini, V. Lupinc, H. Watt, University Edinburgh, UK, 1999,
pp. 109–118.
Fig. 5 shows experimental creep curves compared with the
[5] P.R. Bhowal, E.F. Wright, E.L. Raymond, Metal. Trans. A 21A
results of the simulation, using the proposed model: creep (1990) 1709–1717.
behavior of U720 CR and U720 HS at 850 and 900 MPa is [6] D. Locq, M. Marty, P. Caron, in: Proceedings of the Superalloys
fairly well predicted, but creep behavior of U720 HS at 750 2000, TMS, Metals Park, OH, 2000, pp. 395–403.
and 800 MPa has to be further analysed. [7] M. Condat, B. Décamps, Scripta Metal. 21 (1987) 607–612.

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