J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.

Microstructural Characterization and Mechanical Properties

of Powder Metallurgy Dual Phase Steel Preforms

K. Mahesh, S. Sankaran† and P. Venugopal

Department of Metallurgical and Materials Engineering, IIT Madras, Chennai, India
[Manuscript received February 19, 2012, in revised form April 6, 2012]

In order to improve the mechanical properties of powder metallurgy (P/M) ferrite–pearlite steel, a dual phase
(DP) ferrite–martensite steel was produced through intercritical annealing of sintered P/M preforms. Mi-
crostructures of the sintered and DP steels were examined with optical, scanning and transmission electron
microscopes. Mechanical properties were evaluated through hardness measurements and compression tests.
Microstructural studies revealed that sintered steel contained polygonal ferrite–pearlite while the DP steel
contained polygonal, lath and acicular ferrite along with lath-type martensite as microstructural constituents.
In DP steels, with increasing mean preform density, the microstructure contained fine and continuous network
of martensite colonies with minimum porosity. The work hardening rate vs plastic strain plots (Jaoul–Crussard
analysis) of both the steels revealed typical three stage deformation behaviour for low and high mean preform
densities. Compression tests revealed that, DP P/M steel displayed higher strength-plasticity combination
than the sintered steel.

KEY WORDS: Powder metallurgy; Dual phase; Jaoul–Crussard analysis; Work hardening rate

1. Introduction increase in the strength is achieved by the addition of

Dual phase (DP) steels are high-strength low-
alloy steels and are characterized by a microstructure
consisting of islands of hard martensite in the soft
ferrite matrix. These steels have a combination of
strength, ductility and formability that make them
attractive for weight-saving applications such as au-
tomobile body panels and brake drums in automo-
bile sector[1,2] . Powder metallurgy (P/M) process is a
versatile and efficient route for producing components
with combinations of various alloying elements. These
alloying elements significantly improve the harden-
ability by shifting the transformation curves to the
longer transformation time. Subsequent heat treat-
ment like intercritical annealing results in enhanc-
ing the mechanical properties of ferrous alloys[3–5] .
To ensure similar properties as those of quenched
and tempered steels, Si and Mn are added to in-
crease the strength of microalloyed steels. Further
† Corresponding author. Assoc. Prof., Ph.D.; Tel./Fax:
+91 44 2257 4776; E-mail address: ssankaran@iitm.ac.in (S.
Sankaran).
V, through the precipitation of vanadium carbides[6] .
It is reported in literature[7] that DP steels, pro-
duced through P/M route, show superior properties
than sintered ferrite–pearlite steels. In DP steels, the
volume fraction of martensite increases with increas-
ing intercritical annealing temperature; thereby, the
strength increases. DP microstructures are complex,
as they consist of mixtures of martensite, retained fer-
rite, epitaxial ferrite, retained austenite and various
types of ferrite-carbide aggregates[8] . In general, with
the increase in cooling rate, the morphology of ferrite
changes from polygonal to plate-type or lath-type or
acicular ferrite[9,10] . When the steel is processed at
low cooling rate, the resultant microstructure con-
tains polygonal ferrite having coarse and fine grain
size distribution. Intermediate cooling rate, produces
elongated ferrite grains with high dislocation density
while high cooling rate promotes predominately lath-
type or bainitic ferrite in the microstructure[11] .
The mechanical behaviour of these DP steels arises
from the process of stress and strain partition
1086 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.
Table 1 Properties of base iron powder
Apparent density Flow rate
2.98 g·cm−3 28.0 s/50 g +212 (0%), −212+180 (1.3%), −180+150(7.2%), −150+45 (Bal.), −45 (20.8%)
between the martensite and ferrite, which brings out
inhomogeneous deformation when an external force
is applied[12] . The stress–strain behavior of DP
steels is possibly represented by as many as three
strain regions and the number of stages depends on
microstructural parameters such as grain size and
martensite volume fraction[13,14] . Single work hard-
ening mechanism may not describe the entire behav-
iour at all strains when more than one stage exists.
So, the Jaoul–Crussard (J–C) approach is used to an-
alyze such a behaviour. Many researchers have at-
tempted to describe the stress–strain or work hard-
ening behaviour of DP steels and it is reported that
two stages of strain hardening are observed with mod-
ified J–C analysis[13,14] . In the region of small strains
(ε ≤0.03), the strain hardening rate is dependent on
martensite volume fraction, while at higher strains
it is not. Using the J–C analysis, the deformation
behavior is divided into three different stages when
martensite content is less than 30%[12] . In order to
describe the mechanical behaviour of P/M preforms,
it is pertinent to study the work hardening behav-
iour of sintered and DP steel of various preform densi-
ties. Also, there are limited studies on the mechanical
behaviour of DP steel produced through P/M route.
Hence the purpose of the present study is to produce
DP steel through P/M route of various mean pre-
form densities and to describe their work hardening
behaviour by J–C analysis with detailed microstruc-
tural characterization. The results are compared with
ferrite–pearlite sintered steel and structure–property
correlations are attempted.
2. Experimental
The materials selected for the present study are
elemental powders of pure iron, carbon, manganese,
silicon and vanadium powders. The basic properties
of elemental iron powder such as apparent density,
flow rate and sieve analysis are listed in Table 1. The
chemical composition of the steel is Fe–0.35C–1.5Mn–
0.5Si–0.09V (in wt%). These elemental powders were
thoroughly mixed for about 45 min and a floating die
compaction tool set up was used for preparing the
compacts of various densities in order to minimize the
density gradient across the length of the compact[15] .
The dimensions of the compacts are 25 mm in di-
ameter and 20 mm in length. Green compacts were
dewaxed at 650 ◦ C for 15 min in nitrogen atmosphere
and subsequently sintered at 1120 ◦ C for 30 min in
dissociated ammonia atmosphere. Sintered samples
were sliced into identical pieces across the length of
the compact and the mean preform density of the
compact was calculated by measuring the geometri-
cal density (mass/volume) of each slice. The average
Sieve analysis/µm
value of these densities is the mean preform density of
that particular compact. The achieved sintered den-
sities for various compacting pressures are presented
in Table 2.
Table 2 Compacting pressures and achieved
sintered densities
Compacting pressure Sintered density
/MPa /g·cm−3
375 5.31
450 6.29
532 6.87
679 7.28
Sintered samples of various densities were sub-
jected to intercritical annealing heat treatment
process at 764±2 ◦ C for 20 min and immediately
water quenched. The intercritical temperatures of
the steel were calculated through Thermocalc soft-
ware. The AC1 and AC3 temperatures of the steel are
696 and 786 ◦ C, respectively. Microstructural stud-
ies were performed on (1) sintered and (2) intercritical
annealed samples. Optical (Leitz laborex 12 ME, Ger-
many) and scanning (FEI Quanta 200, USA) electron
microscopes were employed to analyse the microstruc-
tural constituents. To reveal the phases in the mi-
crostructure, 2% nital etching solution was used. A
systematic point count method was used to calculate
the volume fraction of different phases and the grain
size was estimated in terms of mean intercept length
(Lα ) by Eq. (1)[16]
Vα × LT
Lα = (1)
Nα
where Vα is the ferrite volume fraction, Nα is the num-
ber of ferrite grains intercepted by the test line and
LT is the total length of the test line. The contiguity
ratios of different microstructural constituents were
calculated by Eq. (2)[17]
2(PL )M−M
CM =
(PL )F−M + 2(PL )M−M
2(SV )M−M
= (2)
(SV )F−M + 2(SV )M−M
where (PL )M−M and (PL )F−M are number of point
intersections per unit length of the test line with
martensite–martensite and martensite–ferrite bound-
aries and (SV )M−M and (SV )F−M are the correspond-
ing surface area per unit volume of these boundaries.
The contiguity ratio varies from 0 to 1. Marten-
site contiguity ratio is a measure of its connectivity
throughout the microstructure. Measurements were
carried out on micrographs taken at five different lo-
cations for each specimen and an average value was
 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.
Fig. 1 Thinning plots of the powder compacts of various
preform densities
obtained. Similarly, the contiguity ratio of the pores
was also estimated. Foils of DP P/M steel of ∼100 µm
in thickness were prepared for transmission electron
microscopy (TEM, Philips CM12, The Netherlands)
studies by mechanical polishing. The thin foils for
TEM observations were prepared employing twin jet
electro polisher with 10% perchloric acid in ethanol
as electrolyte. Compression tests were conducted on
both steels in order to obtain the flow curves. In the
case of P/M components where porosity is inherent,
the work-hardening takes place due to the metal ma-
Fig. 2 Optical micrographs of sintered P/M steel with varying mean preform densities: (a) 5.31 g·cm−3 ,
(b) 6.29 g·cm−3 , (c) 6.87 g·cm−3 , (d) 7.28 g·cm−3 . P—porosity, grey conveys presence of pearlite and
white represents ferrite phase
1087
trix and also as a result of pore closure. Thus, plastic
properties of P/M are represented as the apparent val-
ues of strength coefficient (Ka ) and strain hardening
exponent (na )[18] .
3. Results and Discussion
3.1 Compacting pressure and thinning plots
Compacts of various densities were produced by
varying the compacting pressure and the variations
in the density level along the length of the compact of
various initial preform densities are shown in Fig. 1.
It can be observed that as the compacting pressure
increases, the density gradient decreases. At lower
pressures poor packing of the particles results in large
pores giving rise to large density variation and with in-
creasing pressure better packing of the particles takes
place. Thus, it is seen that at higher compacting pres-
sures uniform compact can be obtained.
3.2 Microstructure
The microstructures of sintered and DP steels of
varying mean preform densities are shown in Figs. 2
and 3. The microstructures reveal that the sintered
steel consists of ferrite–pearlite while the DP steel
consists of ferrite–martensite as microstructural con-
stituents. It can be observed that the porosity level
decreases and the connectivity of martensite phase
1088 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.

Fig. 3 Optical micrographs of DP P/M steel with varying mean preform densities: (a) 5.31 g·cm−3 ,
(b) 6.29 g·cm−3 , (c) 6.87 g·cm−3 , (d) 7.28 g·cm−3 . P—porosity, M—martensite and F—ferrite phase

Fig. 4 Bright field TEM micrographs showing martensite morphology in DP P/M steel: (a) lath martensite on
the grain boundary in the polygonal ferrite matrix, (SAED patterns obtained in the region denoted as A,
B and C in (a)), (b) high magnification image of the lath-type martensite
 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.
increases with increasing mean preform density. This
supposes that, due to the interconnected porosity and
large porosity fraction the grain boundaries are at-
tached to pores in low mean preform densities. Hence,
the effective grain boundary surface area available for
austenite nucleation is restricted by porosity. The
austenite that nucleates in the highly porous steel
later transforms to martensite upon quenching, and
here the austenite nucleation rate is less than the
growth rate because of restriction by pores. Thus,
martensite forms as large grains heterogeneously. At
high mean preform densities, the grain boundaries get
separated from pores and the effective grain boundary
surface area is larger[19] . Thus, the austenite nucle-
ation rate is higher than the growth rate and the fine
austenite grain transforms to fine colonies of marten-
site in a continuous manner. The volume fraction of
porosity level decreases with increasing mean preform
density of sintered and DP steel.
Bright field TEM micrographs of DP steel re-
veal the martensite morphology in ferrite matrix as
shown in Fig. 4. It is evident from Fig. 4(a) that
lath-type martensite is formed on the grain bound-
aries besides the polygonal ferrite. The selected area
diffraction (SAED) patterns obtained in the region
denoted as A, B and C in Fig. 4(a) are also pre-
sented. The indexed pattern reveals that the marten-
site phase displayed two orientation relationship with
ferrite [112]M //[111]F and [013]M //[111]F in the re-
gion A of Fig. 4(a). The diffraction pattern obtained
from region B displayed orientation of two closely
martensite laths parallel to each other (within 5 deg.)
and the diffraction pattern obtained from the region
C displayed [111] orientation of ferrite. Fig. 4(b) is a
high magnification micrograph of lath martensite. In-
terestingly, lath-type and acicular type morphologies
of ferrite are observed apart from polygonal ferrite in
DP steel as it is evident in Fig. 5. Bright field TEM
micrographs showing lath-type ferrite morphologies
and the dislocation substructures in the ferrite ma-
trix of the DP P/M steel are shown in Fig. 5(a) and
(b) and the indexed SAED patterns obtained in the
region denoted as A, B and C in Fig. 5(a) are also
presented. The diffraction pattern analysis revealed
that the ferrite region denoted as A and B exhibit
predominately [111] orientation. The above analysis
suggests that the ferrite microstructure contains large
number low angle grain boundaries and also the steel
exhibits a kind of local texture or mesotexture.
These findings emulate typical microstructural
characteristics of thermomechanically processed
steels[20] . In general the microstructure is complex
and consisted of non-equiaxed or quasi-polygonal
ferrite, lath-type (bainitic) ferrite and acicular fer-
rite in addition to lath-type martensite. The above
mentioned non-equilibrium ferrite morphologies are
the typical characteristics of continuously cooled mi-
crostructures. The quasi-polygonal ferrite is the first
high temperature phase that forms during continuous
1089
cooling. It forms via a reconstructive mechanism in-
volving diffusion of atoms and grows, initially, along
the austenite boundaries[20] . Acicular ferrite forms
at intermediate temperatures and its growth occurs
through a diffusionless and displacive mechanism in-
volving carbon partitioning in the austenite. Bainitic
or lath-type ferrite also forms at intermediate tem-
peratures similar to acicular ferrite displacive mecha-
nism. However, its morphology is different from the
acicular because of repeated formation of subunits to
generate lath morphology[20] .
Similar kind of lath-type ferrite micrographs
are reported in literature[20] when Nb- and V-
microalloyed steels are processed at high cooling rate.
Illustrations of the precipitates of carbonitrides in the
ferrite matrix in the order of 10–15 nm in polygonal
ferrite are presented in Fig. 6(a). These fine carboni-
tride precipitates effectively pin (Fig.6 (b)) the dis-
locations and provide resistance to dislocation move-
ment. The fine precipitates of vanadium carbonitrides
in the ferrite matrix are formed during cooling and
the precipitation of microalloying elements also occurs
during various stages of thermomechanical processing
of steels[6] .
It is evident from Fig. 7 that the decrease in the
connectivity among pores increases the grain bound-
ary surface area, which in turn increases the marten-
site connectivity and decreases the ferrite grain size.
Thus, with increasing mean preform density, the grain
boundary surface area increases and the ferrite grain
size (in terms of mean intercept length) decreases,
which results in an increase of the strength of the DP
steel. Fig. 8 shows the SEM micrograph of high den-
sity sintered and DP steels, which reveals the pearlite
morphology and martensite connectivity in ferrite ma-
trix. The variation in the hardness of sintered and DP
steel is presented in Fig. 9. The plot reveals that due
to the presence of martensite, the hardness of DP steel
showed superior values than sintered steel for various
densities.
3.3 Compression test
Standard compression tests have been performed
till rupture on cylindrical samples of sintered and DP
steels with aspect ratio approximately equal to 1. The
typical stress–strain plots for varying preform den-
sity are shown in Fig. 10. In order to understand
the deformation behaviour of DP steel, work harden-
ing rate (dσ/dεp ) has been evaluated. Plots of work
hardening rate as a function of true plastic strain of
low (5.31 g·cm−3 ) and high (7.28 g·cm−3 ) mean pre-
form densities of sintered and DP steels are shown in
Fig. 11. The elastic strain has been subtracted from
the total strain for attaining the true plastic strain. At
low mean preform densities, even though the strength
of the DP steel is slightly higher than the sintered
steel, the amount of strain accommodated is less as
compared to sintered steel. It is supposed that, the
1090 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.

Fig. 5 (a) Bright field TEM micrographs showing different ferrite morphologies and the dislocation substructures
in the ferrite matrix of the DP P/M steel, SAED patterns obtained in the region denoted as A, B and C,
(b) bright field TEM micrographs displaying the predominant lath-type or acicular type ferrite and the
dislocation substructures in the microstructure of dual phase P/M steel

heterogeneous distribution of martensite resists the 3.4 Work hardening behaviour (Jaoul–Crussard
uniform deformation because in high density preform, analysis)
the increase in the connectivity and fine morphology
of martensite in ferrite matrix promotes the strength- The description of work hardening behaviour using
plasticity combination. the log(dσ/dεp )–log(εp ) plot is called Jaoul–Crussard
 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094. 1091

Fig. 6 Bright field TEM image of DP steel showing carbonitride precipitates of vanadium in the polygonal ferrite

Fig. 7 (a) contiguity ratio and (b), surface area per unit volume and ferrite grain size against mean preform
density of DP steel

Fig. 8 SEM micrographs showing pearlite morphology in sintered steel (a) and martensite connectivity in DP
steel (b)

(J–C) analysis. The plots exhibit stage behaviour
of work hardening rate as a function of true plas-
tic strain, which is generally observed in multiphase
materials such as DP steels, Cu–Al alloys[21] . In the
present study both the sintered and DP steels display
three stage work hardening behaviour in J–C plots at
low and high preform densities (Fig. 12(a)–(d)). A
linear fit has been obtained using Lüdwik equation in
order to determine Lüdwik parameters (Ka and na
values) corresponding to three linear segments. The
Ka and na values of sintered and DP steels for differ-
ent stages are presented in Table 3.
For fully dense materials, the stage behavior is
normally correlated to changes in the microstructures
during deformation. For porous materials, in addi-
tion to microstructural aspects, the role of porosity
and impurity oxides are also to be considered in un-
derstanding the deformation behavior. The P/M pre-
forms of sintered and DP steels with low densities,
display high na and low Ka values in stage I as com-
1092 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.
Fig. 9 Hardness variation of sintered and DP steel of
varying densities
pared to stage II, while in stage III, both na and Ka
values are negative. Considering the Lüdwik parame-
ters for three stages, the stage I behavior is related to
predominant pore closure/flattening (high na ) in ad-
dition to the matrix hardening. The stage II is char-
acteristic of non-uniform deformation and related to
predominant matrix hardening (high Ka ) in addition
to pore closure/flattening. Stage III behavior is ex-
pected primarily due to pore coalescence, breaking of
brittle martensite/pearlite phase and dynamic recov-
ery effects till fracture. It may be noted that in low
Fig. 10 True stress–true strain plots of sintered (a) and DP (b) steels of varying densities
Fig. 11 True stress and work hardening rate as a function of true plastic strain of sintered (a) and DP (b) steels
preform density DP steel, even though the marten-
site is present in similar fraction as high density steel,
there is only a marginal increase in the strength as
compared to sintered steel. This is possibly due to
the heterogeneous distribution of the coarse marten-
site phase in the ferrite matrix, which resists the uni-
form deformation.
The Lüdwik parameters of sintered and DP steels
with high preform density are different from the low
density steels. The stage I is characterized by high
na value as compared to stage II in both the steels.
However, in sintered steel, Ka value in stage I is low
compared to stage II while DP steel displays similar
Ka values in both stages. In stage III, both steels
exhibit negative values of Lüdwik parameters. In sin-
tered steel, stage I deformation is due to pore clo-
sure/flattening and ferrite matrix deformation while
in stage II it may be due to the combined effect of
ferrite and pearlite deformation, which is indicated by
its high Ka value. In DP steel, it is believed that the
stage I deformation is associated with the combined
effect of ferrite and martensite phases apart from pore
closure/flattening (as indicated by high Ka and na
values).
This effect is primarily related to the presence of
fine martensite phase, which is homogeneously dis-
tributed with high connectivity in ferrite matrix. The
stage II deformation is related to ferrite–martensite
 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094. 1093

Fig. 12 Work hardening rate showing a typical three stage behaviour of low ((a) and (c)) and high ((b) and (d))
mean preform densities of sintered ((a) and (b)) and DP ((c) and (d)) steels

Table 3 Lüdwik parameters of sintered and DP steel in different stages

Sintered steel DP steel
5.31 g·cm−3 7.28 g·cm−3 5.31 g·cm−3 7.28 g·cm−3
σ0 35±8 86±14 14±4 106±12
Stage I na 0.833±0.05 0.404±0.08 0.642±0.05 0.604±0.07
Ka 453±16 544±25 474±18 815±27
σ0 – – – 38±21
Stage II na 0.617±0.07 0.327±0.04 0.590±0.08 0.494±0.09
Ka 485±15 686±12 494±19 813±25
σ0 359±14 468±13 272±18 888±21
Stage III na –0.806±0.04 –0.124±0.07 –0.796±0.08 –0.960±0.06
Ka –34±11 –32±17 –30±22 –138±27

with the martensite deformation dominating over fer-
rite. For a fully dense material, stage I is usually
characterized by an inhomogeneous dislocation dis-
tribution, which becomes more uniform towards the
end of the stage I and stage III is associated with
the cross slip and dynamic recovery effects[22] while
stage II reflects the uniform elongation[14] . Similar
kind of observations are reported in literature[6,22,23]
reporting the negative values of K and n in stage III.
It is reported in literature[14] that DP steel exhibits
three deformation stages when martensite is present
in the matrix, even in small amounts but such defor-
mation behaviour disappears if the martensite content
is greater than 30%[12] . From the above discussion, it
may be supposed that the P/M DP steel derives the
possible strength–toughness combination from the fol-
lowing: (1) fine lath-type martensite and its high con-
tiguity ratio; (2) lath-type and acicular ferrite mor-
phologies; (3) high dislocation density and its sub-
structures; (4) vanadium carbonitrides precipitation
in the ferrite and their pinning with dislocations.
4. Conclusions
(1) Dual phase (DP) ferrite–martensite P/M steels
have been produced through intercritical annealing
of sintered ferrite–pearlite P/M preforms of differ-
ent mean preform densities. The microstructure of
processed steels contained about 20%–28% marten-
site.
1094 K. Mahesh et al.: J. Mater. Sci. Technol., 2012, 28(12), 1085–1094.
(2) In high mean preform density DP steels, the
martensite morphology was fine and it formed a net-
work in the ferrite matrix with high connectivity in
comparison to low mean perform density steels.
(3) The high density DP steel displayed high
strength and plasticity than the sintered steel. Pres-
ence of a mixture of quasi-polygonal, lath-type or aci-
cular ferrite along with fine lath-type martensite of
high contiguity ratio in the microstructure promotes
superior strength-plasticity combination in DP P/M
steel.
(4) Work hardening behaviour (J–C analysis) of
both DP and sintered steels revealed typical three
stage behavior. However, the DP P/M steel exhib-
ited uniform work hardening behavior as opposed to
the sintered steel.
Acknowledgements
The authors are very thankful to Mr. Gopinath for
permitting to use the industrial sintering furnace. The
authors also acknowledge Mr. Papa Rao for his kind help
in TEM work.
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