Materials Science and Engineering A 550 (2012) 97102

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Materials Science and Engineering A
j our nal homepage: www. el sevi er . com/ l ocat e/ msea
Effect of heat treatment on microstructure and mechanical properties of laser
melting deposited Ni-base superalloy Rene

41
J. Li, H.M. Wang

, H.B. Tang
Laboratory of Laser Materials Processing and Manufacturing, Beihang University (formerly Beijing University of Aeronautics and Astronautics), 37 Xueyuan Road,
Beijing 100191, China
a r t i c l e i n f o
Article history:
Received 3 February 2012
Received in revised form29 March 2012
Accepted 8 April 2012
Available online 13 April 2012
Keywords:
Rene

41
Laser melting deposition
Standard heat treatment
Mechanical properties
a b s t r a c t
Ni-base superalloy Rene

41 was produced by the laser melting deposition (LMD) manufacturing process.

The LMD material was solution treated at 1065

C for 4h followed by air quenching and aged at 760

C
for 16h followed by air cooling. Microstructure of the as-deposited, solution treated and solution-aged
alloys were characterized by scanning electron microscopy and transmission electron microscopy, and
the tensile properties and hardness were tested. The solution-aged Rene

41 superalloy showed high

hardness, low strength and low ductility. The extensive precipitation of

resulted in high hardness

and ductility, and the subsequent alignment and coalescence of

precipitates induced low strength.

The structureproperty relationships of the alloy under three different heat treating conditions were
studied and results indicated that the standard heat treatment recommended for wrought Rene

41 was
not suitable for LMD alloy and had to be modied to realize optimum mechanical properties.
2012 Elsevier B.V. All rights reserved.
1. Introduction
Rene

41 is a nickel-base superalloy developed as a high-

strength, high temperature material in the mid-1950s based on
its good tensile strength and creep-rupture strength combined
with an excellent oxidation resistance at the range of 650900

C.
It has been widely used for hot section parts in aircraft engines
[13]. However, a high tendency of cracking during forging and
welding restricts its use, which is due to its bad thermoplas-
ticity and serious segregations during conventional slow-cooling
casting process. Laser melting deposition (LMD) is a layerwise
rapid solidication material additive manufacturing technology
which builds complex-shaped components froma computer-aided
design model [4,5]. The technology offers considerable cost sav-
ings, since extensive machining and welding processes are not
involved. Laser melting deposited Rene

41 was preferred due to its

improvedhomogeneity andner microstructure resulting fromthe
rapid solidication cooling rate. The microstructure and mechan-
ical properties of as-deposited alloy was previously studied and
reported elsewhere [6].
Rene

41is aprecipitation-hardenedsuperalloy, andits strength-

ening mechanism depends on the size and the morphology of
gamma prime phase and carbides, both of which are affected by
heat treatment. In order to improve the mechanical properties, the

Corresponding author. Tel.: +86 10 8231 7102; fax: +86 10 8233 8131.
E-mail address: wanghm@buaa.edu.cn (H.M. Wang).
LMD Rene

41was solutiontreatedat 1065

Cfor 4h/air quenchedto

roomtemperature and then aged at 760

C for 16h/air cooled. The

microstructureandmechanical properties of as-deposited, solution
treated and solution-aged material were discussed in this paper.
2. Experimental
The commercially available, vacuum non-contacting plasma
melting argon atomized Rene

41 powders were used in this

study, and the detailed parameters of the LMD process have been
reported elsewhere [6]. The LMD alloy was given a solution treat-
ment at 1065

C/4h/air quenched to room temperature followed

by an aging treatment at 760

C/16h/air cooling. Metallographic

samples (two samples for each condition) were mechanically
polished and etched in a chemical solution of 3g CuSO
4
, 80ml
HCl, 20ml absolute alcohol and were immersed in ammonium
peroxydisulfate:H
2
O solution in weight ratio of 1:20 for several
minutes to remove corrosion products. Microstructure of samples
were characterized by JSM-5800, eld emission high resolution
scanning electron microscopy S4800 and Cambridge-S360 (SEM)
equipped with League-2000 energy dispersive spectroscopy (EDS).
As the quantitative metallographic investigation is basically a
statistical measurement, a large number of images at different
magnications were analyzed with only one of each is shown here.
The carbon extraction replica technique was used to prepare sam-
ples to identify the interdendritic phase precipitated during the
aging treatment by JEM-2100F transmission electron microscopy
(TEM). This technique consistedof a single-stage carbonextraction.
0921-5093/$ see front matter 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2012.04.037
98 J. Li et al. / Materials Science and Engineering A 550 (2012) 97102
Fig. 1. Microstructure of the as-deposited Rene

41 superalloy.
A carbon layer is sputtered on the specimen surface and then an
etching procedure (
1
HF:
7
HNO
3
etching solution) was performed
in order to collect the replicas. The hardness of the samples was
measured using a Vickers microhardness tester using a 1000g load
for a dwell time of 18s. The average hardness value was calculated
from eight indentations. Room temperature tensile tests were
performed on a MTS880 universe tensile testing machine using
column tensile test specimens with a diameter of 5mm and a
gauge length of 25mm. The reported tensile data are an average
of three test results. The surfaces of the failed specimens were
examined by SEMto study the fracture characteristics.
3. Results
3.1. Microstructure
The microstructure of the as-deposited alloy Rene

41 (Fig. 1)
consisted of ne rapid directionally solidied columnar grains with
some ne MC carbide particles distributed in the interdendritic
areas. The MC carbides were found to be enriched in Ti and Mo.
The size of

precipitates in the dendritic cores was larger than

that in the interdendritic zones, and possible reasons for this have
been discussed elsewhere [6].
The solution treatment has been applied to dissolve the coarse

and MC carbides formed during solidication and to reduce the

chemical segregation due to partitioning of some of the elements
to the interdendritic regions. The microstructure of the solution
treated alloy presented in Fig. 2 revealed that the austenite matrix
contained un-dissolved

particles, MC carbides and ultrane re-

precipitated

particles. The solvus temperature for

in Rene

41
has been reported to be 1065

C [7], however, it was clear from

Fig. 2 that 4h solution treatment at 1065

C was not sufcient to

dissolve all the coarse

particles. The splitting of

particles was
visible under higher magnications as indicatedinFig. 2b, andmost
of the un-dissolved

particles possessed near-cubic morphology

and tended to grow to split into smaller ones from their edges
of the initial precipitate toward its center. A detailed description
of a similar splitting process phenomenon was given by Grosdi-
dier [8]. According to the micrograph and the EDS analyses, the
near-equiaxed or script-like MC carbides decreased after solution
treatment. In addition, the columnar grains which resulted from
laser melting depositionprocess remainedapproximately the same
as that of the as deposited alloy. Transformation from columnar
grains to equiaxed grains which was reported elsewhere [9] was
absent here. Althoughgrainboundaries of the solutiontreatedalloy
Fig. 2. Microstructure of the as-deposited Rene

41 superalloy after solution treat-

ment at 1065

C for 4h and cooled in air: (a) un-dissolved

particles and carbides,

and re-precipitated

particles, (b) splitting of some coarse

particles and hyper-

ne re-precipitated

particles.
were not easy to etch clearly, the solution and aged alloy revealed
the columnar grain morphology clearly.
The solution treated alloy was given an ageing treatment. Fig. 3
showed the microstructure of the aged alloy consisting of

parti-
cles in different sizes, MC carbides and some other interdendritic
phases which precipitated in the ageing treatment. The interden-
dritic phases were equiaxed or strip-shaped and had an average
length of approximately 300600nm (Fig. 3b and c). According
to the composition and selected area diffraction (SAD) pattern
(Fig. 3d), it could be inferred that the particles were mainly M
23
C
6
,
where Mrepresented Cr and Mo. The precipitation of the discrete
M
23
C
6
carbides was caused by carbide reactions during the aging
at 760

C for 16h. During aging at 760

C for a relatively long time,

there was enoughtime for the formationof M
23
C
6
carbides through
carbon diffusion and reaction with the Cr and Mo. Furthermore, it
is believed that M
6
C carbides which have a complex cubic struc-
ture similar to M
23
C
6
were inclined to formduring aging partially
replacing M
23
C
6
when the Mo content is high [10]. Since the Mo
content is 910wt% in Rene

41 alloy, the interdendritic phases

might be the mixture of M
23
C
6
and M
6
C.
During aging at 760

C, in addition to an increase in their mean

size, the

particles also underwent a change in morphology

(Fig. 4). The cuboidal

precipitates tended to group together in

short chains or blocks of several particles and coalescence subse-
quently (Fig. 4c and e). The TEMmicrograph in Fig. 4d showed the
interface of the and coarsened

was covered by an interfacial

J. Li et al. / Materials Science and Engineering A 550 (2012) 97102 99
Fig. 3. Microstructure of LMD Rene

41 superalloy after solution and ageing treatment: (a) the columnar grain morphology, (b) different sizes of

particles, MC and M23C6

carbides, (c) bright eld image showing the M
23
C
6
carbides, (d) SAD pattern corresponding to the carbides in (c).
dislocation network. Size and morphology of

precipitates in
different conditions were given in Table 1 for a clear comparison.
3.2. Tensile properties and hardness
The room temperature tensile properties of alloy Rene

41 in
the as-deposited, solution treated and solution-aged conditions
and a minimum allowable specication for Rene

41 as aeronau-
tical material [3] were given in Table 2. These results indicated
that after solution treatment, there was a drastic decrease in yield
strength (YS) and ultimate tensile strength (UTS) compared to the
as-deposited material while substantial improvement took place
in both the elongation (EL) and reduction in area (RA). In contrast
with the solution treated alloy, alloy in solution-aged condition
showed improvement of YS and UTS, but considerable drop in EL
and RA. Microhardness of samples under three different conditions
in Table 2 revealed that the hardness varied obviously, and both
the as-deposited and the solution-aged alloy showed considerable
high microhardness values compared to the minimum allowable
specication, with samples after solution-aged showed the highest
hardness. In conclusion, LMD Rene

41 alloy which experienced the

standard heat treatment recommended for wrought Rene

41 failed
to meet the minimum allowable specication, with higher EL, RA
and microhardness but lower YS and UTS.
3.3. Fractography and sub-surface of fracture
The fracture surfaces of the solution treated alloy as well as
the solution-aged material were examined by SEM. The solution
treated material showed homogeneous deformation and fully dim-
pled rupture (Fig. 5), suggestive of a transgranular ductile mode of
failure responsible for the high value of elongation of about 42.2%.
In contrast to the solution treated alloy, the fracture sur-
face of the solution-aged material showed that lots of secondary
cracks (Fig. 6a) followed the columnar grain boundaries apparently
(Fig. 6b), moreover, thesurfacecontainedconsiderablenedimples
(Fig. 6c), the size of which is close to that of coalesced

, that is,
chains or blocks of several

. Note that the crack propagated along

the interface between and coalesced

(Fig. 6d).
Table 1
Size and morphology of

precipitates in different conditions.

Material condition Volume fraction (vol.%) Average size or length (nm) Morphology
As-deposited 2327 25050 Big and small cuboids
LMD +solution treated 57 120170 (average size of small
ones after splitting)
Some coarse

particles are splitting

into smaller ones while some other
ultrane

precipitates
LMD +solution-aged (16h) 7001700 (average length of
chains or blocks)
Short chains or blocks of several
particles
100 J. Li et al. / Materials Science and Engineering A 550 (2012) 97102
Fig. 4. Micrographs of

phases in alloy solution treated at 1065

C for 4h and subsequently aged at 760

C for (a) 12h, (b)14h, (c) 16h, showing short chains or blocks of
several particles which was induced by the coalescence of adjacent

precipitates, (d)16h, and TEMmicrograph showing dislocations at /coarsened

interface, (e) 18h.

4. Discussion
The as-deposited LMD Rene

41 superalloy consisted mainly of

a Ni-base austenitic matrix,

precipitate and near-equiaxed or

script MC carbides. After solution treatment, some

dissolved
while some other coarse

failed to dissolve and grew to split.

The splitting of coarse

precipitates into a number of small par-

ticles or cuboids during cooling or long time ageing has been
observed in other Ni-base alloys [8,11,12] and the mechanism of
the splitting phenomenon has not been completely clear. Some
researchers [13,14] suggested it was an elastically driven process
while other calculations showed the interface instability driven by
elastic anisotropy and diffusion eld generated particle splitting
[15]. Furthermore, a small amount of ultrane

re-precipitated
during cooling due to the reduction of solubility of Ti and Al in
matrix. However, no other types of carbides were detected after
solution treatment though a portion of MC carbides dissolved dur-
ing the process. This couldbe attributedto the highcooling rate and
the relatively sluggish precipitation dynamics of M
23
C
6
compared
to the relatively fast continuous precipitation kinetics of

phase.
The solution treated material then underwent an ageing treat-
ment and several microstructure changes occurred. The process
of growth of

precipitates seemed to occur through coalescence

of adjacent

particles, and the

precipitates inclined to group

together in short chains or blocks of several particles and coa-
lescence subsequently. The tendency for

precipitates to form
raft-like microstructures in the absence of applied stress was
reported in several alloys and was related to the magnitude of
the mist between

particles and matrix [1619]. In addition to

the changes of

precipitates, M
23
C
6
carbides precipitated during
aging treatment due to the dissolution of partial MC carbides and
the release of C to the matrix.
Table 2
Mechanical properties and hardness of alloy Rene

41 evaluated at roomtemperature.
Material condition 0.2%YS (MPa) UTS (MPa) %EL %RA Hardness (HV)
As-deposited 8529.4 111735.1 212.5 22.71.5 426.588.5
LMD +1065

C/4h/AC 56327.3 83840.3 42.26.8 38.76.3 261.6325.2

LMD +1065

C/4h/AC +760

C/16h/AC 83510.4 108330.8 124.1 20.88.2 448.810.7

Wrought +1065

C/4h/AC +760

C/16h/AC
a
[3] 880 1175 12 12 400
a
The minimumallowable specication in manuscript.
J. Li et al. / Materials Science and Engineering A 550 (2012) 97102 101
Fig. 5. Fractographs of the solution treated Rene

41 superalloy tested at roomtem-

perature: (a) overall viewand (b) high magnication viewshowing dimple-ductile
fracture.
Thetensileproperties andhardness of thealloyinthreedifferent
conditions were compared to correlate the fracture characteris-
tics with microstructure. The low strength values and hardness
associated with high ductility of the solution treated alloy were
obviously due to the dissolution of

during solution treatment.

The matrix became much softer and the softer matrix could relax
the stress concentration at the interface of two phases which was
believed to be the origin and propagation paths of cracks to frac-
ture. This delayed the fracture and allowed the material to deform
well and nally led to a transgranular mode of failure. It could
be seen that the YS and UTS of the alloy were partially increased
through ageing treatment but were still lower than that of the as-
deposited alloy. Moreover, the ageing treatment brought a huge
drop to the EL and RA. The improvement in the YS and UTS was
attributed to the extensive precipitation of

, which also resulted

in the increase of hardness. However,

particles aligned parallel

to each other to minimize mist stress and coalesced subsequently
to reduce interface area. Meanwhile, the alignment and coars-
ening described above widened matrix corridors and facilitated
the movement of dislocation [16]. Coherency of

interface
became lost when the particles attained a certain size, and the
energy associated with the strained interface became too high,
thus the original ordered interface was replaced by a disordered
interface and interfacial dislocation networks formed. Generally,
strength of alloy was governed by the inverse of interparticle
spacing [20]. The increase of spacing between the coarsened

resulted in low strength. The deformation was localized at the

interfaces and decohesion contributing to microvoid nucleation
occurred. Fromfracture surface observations, it could be seen that
the morphology consisted of ductile regions with considerable ne
dimples.
Fig. 6. Fractographs of the solution-aged Rene

41 superalloy tested at room temperature: (a) overall view showing lots of secondary cracks and (b) revealing that the
secondary cracks follow the columnar grain boundaries, (c) high magnication view showing considerable ne dimples, (d) sub-surface of fracture revealing that the crack
propagated along the interface between and coalesced

.
102 J. Li et al. / Materials Science and Engineering A 550 (2012) 97102
5. Conclusions
The extensive precipitation of

particles during heat treat-

ment resulted in high hardness and ductility, but the subsequent
alignment and coalescence of

precipitates induced decrease in

strength. This suggests that the recommended standard heat treat-
ment for wrought Rene

41 alloy is not suitable for the LMD alloy

for optimummechanical properties.
Acknowledgements
This research was supported by National Natural Science Foun-
dation of China (Grant No. 50671004), National Outstanding Youth
Science Foundation of China (Grant No. 50625416), Cheung Kong
Scholars Innovative Research TeamProgramof Ministry of Educa-
tion(Grant No. IRT0805), State KeyBasic ResearchProgramof China
(Grant No. 2006CB605206).
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