International Journal of Minerals, Metallurgy and Materials

Volume 18, Number 5, October 2011, Page 557

DOI: 10.1007/s12613-011-0477-y
Corresponding author: Abbas Mahmudi E-mail: abbas_5566@yahoo.com
University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg 2011


Effects of cold rolling on the microstructure and mechanical properties
of Fe-Ni-Mn-Mo-Ti-Cr maraging steels

Abbas Mahmudi
1)
, Syamak Hossein Nedjad
2)
, and Mir Masud Jabbari Behnam
3)

1) Young Researchers Club, Islamic Azad University (Ahar Branch), 54516 Ahar, Tabriz, Iran
2) Faculty of Materials Engineering, Sahand University of Technology, Tabriz 51335-1996, Iran
3) Department of Materials Science and Engineering, Sharif University of Technology, Tehran 11365, Iran
(Received: 5 August 2010; revised: 27 September 2010; accepted: 10 October 2010)

Abstract: Effects of cold rolling on the microstructure and mechanical properties of Fe-Ni-Mn-Mo-Ti-Cr maraging steels were studied. To
investigate the microstructure and mechanical properties, optical microscopy, scanning electron microscopy, X-ray diffraction, tensile test,
and hardness test were used. The results show that the solution-annealing treatment in the cold-rolled steel redounds to the formation of sub-
microcrystalline Fe
2
(Mo, Ti) Laves phase particles, which are stable at high temperatures. These secondary Laves phase particles prevent
from recrystallization at high temperatures and correspond to semi-brittle fracture in the subsequent aging treatment.
Keywords: maraging steel; cold rolling; age hardening; Laves-phase; microstructure; mechanical properties



1. Introduction
Since 1960, 18Ni maraging steels have been widely used
for high-performance military and aerospace applications
[1]. After solution annealing in the austenitic state, these
steels transform to lath martensite in subsequent non-equi-
librium cooling conditions [2]. Strengthening of maraging
steels takes place in the precipitation of metastable intermet-
allics during appropriate aging of martensite [3]. The com-
mercial grades of these steels are 18Ni maraging steels with
and without Co content, which are expensive because of
their alloy contents [4]. Extensive researches have been car-
ried out on the development of low-cost maraging steels
with an optimum chemical composition through the substi-
tution of nickel by cheaper elements like manganese, which
results in the invention of Fe-Ni-Mn maraging steels [5].
The Fe-Ni-Mn maraging steels have high capability to be
age hardened, and they have the great potential to be re-
placed with 18Ni maraging steels in respect to high strength
[6]. These steels suffer from premature brittleness in the
grain boundaries of primary austenite after aging treatment
[7]. Segregation of Mn [8] and Ni-Mn intermetallics pre-
cipitation [9] can be accounted for mentioned brittleness.
Different investigations have been done to reduce the grain
boundary brittleness in these steels, in which the addition of
molybdenum, titanium, tungsten, boron, and chromium can
be implied [10-14]. The study by Heo and Lee [14] showed
that chromium addition up to 3wt% led to the development
of strength and toughness. The aim of this paper was to in-
vestigate the effects of cold rolling on the microstructure
and mechanical properties of Fe-Ni-Mn-Mo-Ti-Cr maraging
steels with 4wt% Cr, processed via cold rolling, solution
annealing, and age-hardening route.
2. Experimental
The Fe-Ni-Mn-Mo-Ti-Cr alloy was prepared in a vacuum
induction-melting furnace at 1 Pa using electrolytic iron,
electrolytic manganese, electrolytic chromium, and pure
nickel shots. Table 1 gives the chemical composition of the
alloy prepared. Bars cut from the cast ingots were encapsu-
lated in quartz tubes under argon gas after evacuation to 10
3

Pa. Homogenizing treatment was performed at 1423 K for
173 ks followed by water quenching. The homogenized bars
were cold-rolled for 50% thickness reduction at ambient
558 Int. J. Miner. Metall. Mater., Vol.18, No.5, Oct 2011

temperature, then solution annealed at 1323 K for 3.6 ks in a
vacuum furnace followed by water quenching. Sheet-type
tensile test pieces were cut according to ASTM A370. Ten-
sile tests were carried out using a universal tensile test ma-
chine at a cross-head speed of 1 mm/min at ambient tem-
perature. Aging treatment was carried out for various time at
753 K in a neutralized salt bath. Hardness measurements
were made using the Rockwell C method under the load of
1470 N. X-ray diffraction (XRD) was carried out using Cu
K

radiation of 0.15410-nm wavelength in a Bruker AXS1

D8-ADVANCE instrument. Optical microscopy (OM) and
scanning electron microscopy (SEM) were used for micro-
structural and fractographic studies.
Table 1. Chemical composition of Fe-Ni-Mn-Mo-Ti-4Cr alloy
wt%
Ni Mn Mo Ti Cr C P S Fe
8.75 5.26 5.07 1.39 4.51 0.03 0.007 0.022 Bal.
3. Results and discussion
Fig. 1(a) shows the solidification microstructures of
Fe-Ni-Mn-Mo-Ti-4Cr maraging steels after casting. It exhib-
its the packets of lath martensite, which is found in maraging
steels typically. However, in combination with lath martensite,
retained austenite and second-phase particles are found in the
interdendritic regions, presumably due to the positive mi-
crosegregation of alloying elements during solidification. Op-
tical micrographs of the solidification microstructure of this
alloy after homogenization, cold rolling, and annealing treat-
ments, hereinafter to be refereed as annealed steels, are shown
in Fig. 1(b). Despite this thermomechanical history provides
the solution-annealed martensite in Fe-Ni- Mn maraging
steels [15], it is found that martensite formation disappears in
the present steel completely, being replaced by a uniform
dispersion of submicrocrystalline second-phase particles in a
matrix without characteristic martensite morphology. The
secondary electrons scanning micrograph of the annealed
steel is illustrated in Fig. 2, representing the formation of
submicrocrystalline second-phase particles.

Fig. 1. Optical micrographs representing microstructures of the studied steel in the form of solidification (a) and after homogeniza-
tion, cold rolling, and annealing (b).

Fig. 2. Electrons scanning micrograph of the annealed steel,
representing the formation of submicrocrystalline second
phase particles.
The X-ray diffractogram (Fig. 3(a)) shows the solidifica-
tion microstructure of the studied steel in which diffraction
lines belonging to the body centered cubic (bcc) iron and the
face centered cubic (fcc) iron are found, verifying the for-
mation of martensite and retention of austenite, respectively.
During the annealing process, as shown in Fig. 3(b), the in-
tensities of fcc diffraction lines decrease except for (220)

.
Decreasing the intensities of other fcc diffraction lines can
be attributed to the elimination of alloying elements mi-
crosegregation during the homogenization and precipitation
of second-phase particles, which depletes alloying elements
from the surrounding matrix during annealing. Therefore,
the martensite start temperature is raised above ambient
temperature and consequently, the volume fraction of aus-
tenite decreases by transforming into martensite. The in-
crease of the intensities of (220)

diffraction lines in the an-

nealed steels implies preferred stabilization of a specific
texture of austenite in the cold-rolled steel, which will be
A. Mahmudi et al., Effects of cold rolling on the microstructure and mechanical properties of Fe-Ni-Mn-Mo-Ti-Cr 559

inherited to annealed microstructure from deformation tex-
ture. Furthermore, two diffraction lines appear after anneal-
ing treatment at the diffraction angles of 2=38 and 41, as
represented in Fig. 3(b). The diffraction lines of (11 2 0) and
(11 2 2) belong to Fe
2
(Mo, Ti)-type Laves phases with hex-
agonal close-packed (hcp) crystal symmetry.
It was identified by energy dispersive X-ray microanaly-
sis that in an Fe-10Ni-5Mn-6Mo-1.5Ti-5Cr-0.5W (wt%)
steel, the second-phase particles contained high molybde-
num and occasionally titanium contents [16], in agreement
with the present X-ray diffraction analysis, denoted the for-
mation of Fe
2
(Mo, Ti)-type Laves phases. Therefore, it is
found that annealed microstructures mainly contain disper-
sions of submicrocrystalline Laves phase particles in the bcc
iron matrix.
Changes in hardness of an annealed steel during isochro-
nal aging for 3.6 ks at 653-1153 K are shown in Fig. 4(a),
indicating a peak hardness at about 753 K. It is significant
that even after high temperature aging, hardness values
higher than HRC 40 are preserved, which is attributed to the
formation of Laves phase particles. Fig. 4(b) represents the
change in hardness of the annealed steel vs. isothermal aging
time at 753 K. The annealed microstructure shows the con-
siderable age hardenability, analogous to the age hardening
of lath martensite in 18Ni and Fe-Ni-Mn maraging steels.
The age hardening is attributed to a second-phase precipita-
tion reaction within the bcc iron matrix, forming nanome-
ter-sized intermetallic compounds like Ni
3
Ti, NiMn, etc.
during isothermal aging at 753 K. For example, a high-mag-
nification view of the aged martensite is shown in Fig. 5(a),
which indicates the dense precipitation of nanometer-sized
second-phase precipitates. A selected-area electron diffrac-
tion pattern (SADP) obtained from the aged martensite is
given in Fig. 5(b). Reflections of the bcc iron matrix with a
variant of a face-centered tetragonal (fct) -NiMn precipitate
are identified, indicating an orientation relationship close to
Kurdjamov-Sachs orientation relationship as (011)
bcc
//(111)
fct
,
[100]
bcc
//[1 1 0]
fct
[17]. The studied steel represents high age
hardenability as well as a higher hardness in the annealed
condition, achieving the values of HRC 40 and HRC 55 in
the annealed and peak-aged conditions, respectively.

Fig. 3. X-ray diffractograms obtained from solidification (a) and annealed (b) steels.

Fig. 4. Hardness changes vs. aging temperature of the cold-rolled steel during isochronal aging for 3.6 ks (a) and aging time of the
annealed steel at the isochronal aging temperature of 753 K (b).
560 Int. J. Miner. Metall. Mater., Vol.18, No.5, Oct 2011


Fig. 5. Microstructures of Fe-10Ni-7Mn-6Cr (wt%) alloy after aging for 0.9 ks at 753 K: (a) high-magnification view within mart-
ensite; (b) SADP of the aged martensite [17] (B is the orientation relationship).
Fig. 6 shows the engineering stress-strain curve of the
studied steel after age hardening to the peak value indicated
at 753 K. The studied steel shows an ultrahigh fracture stress
of about 1800 MPa with a negligible tensile ductility.

Fig. 6. Engineering stress-strain curve of the studied steel af-
ter age hardening to the peak value indicated at 753 K.
The scanning electron micrograph obtained from the
fracture surfaces of broken tensile test pieces of the studied
steel is shown in Fig. 7. The arrow head indicates Laves
phase particles, representing both fragile characteristic and
interface decohesion with the surrounding matrix. The mi-
crograph represents fibrous fracture surfaces, which are
recognized with the ductile dimpled fracture with narrow
dimples and the macroscopic irregularities resembling de-
tachment of pancake grains inherited by cold rolling.
4. Conclusions
Cold rolling and solution annealing of homogenized
Fe-Ni-Mn-Mo-Ti-4Cr maraging steels result in the forma-
tion of Fe
2
(Mo, Ti)-type Laves phases dispersed in a bcc

Fig. 7. Scanning electron micrograph obtained from the
fracture surfaces of broken tensile test pieces.
iron matrix, in contrast to 18Ni and Fe-Ni-Mn steels obtain-
ing lath martensite in a similar route of processing. Main
characteristics of the cold-rolled and solution annealed mi-
crostructures are drawn as follows.
(1) The proposed processing leads to the formation of
submicrocrystalline Laves particles that have good stability
at high temperatures.
(2) The studied alloy with the proposed processing rep-
resents high age hardenability.
(3) Ultrahigh fracture stress but poor tensile ductility is
obtained after substantial age hardening.
(4) Cold rolling and subsequent annealing result in the
dispersion of Laves phase particles in the matrix and prevent
the formation of grain boundary precipitations.
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