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Materials Today: Proceedings 18 (2019) 4860–4868 www.materialstoday.com/proceedings

ICMPC-2019

A Study of the Low-Temperature Property of Nodular Iron

S.Shamaa, V.Bramarambaa*, S.Sena
a
Department of Metallurgical and materials Engineering
National Institute of Technology, Rourkela-769008, Odisha, India

Abstract

The Spheroidal graphite Iron (S.G.Iron), (also known as Ductile or Nodular iron) is, presently being used for so many purposes.
In the present work, efforts have been made to find out to what extent the material can be used at sub-zero temperatures. In order
to investigate the low temperature applicability of S.G.Iron the effect of temperature on its impact properties has been studied
with a view to finding out whether it can retain its impact strength even at sub-zero temperatures (-20°C). S.G.Iron with
austenitic and ferrito-pearlitic matrix are used for the experiment and the variation of toughness with temperature has been
studied to examine their utility for low temperature uses.

© 2019 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the 9th International Conference of Materials Processing and Characterization, ICMPC-2019

Keywords: S.G.Iron; ferritic/pearlitic matrix; austenitic matrix; toughness; tensile strength; fractrography.

1. Research background

S.G.Iron also known as Ductile or Nodular Iron was discovered in 1943 by Keith Millis later it was patented in
1948 [1]. Intensive work for the development of the material was first carried out in the decade of 1950s. This led to
exceptional increase in its usage as an engineering material during 1960s. Austenitic S.G.Iron is produced by adding
an austenitic stabilizing element (mostly Ni) to a considerable extent to the melt. The Ni-resist Iron is the most
common grade of Austenitic Ductile (or S.G) cast iron. It contains 12 to 36 % Ni; which is of lesser cost than
alloyed steel [2]. Since the austenitic matrix provides better ductility and toughness than other matrices (e.g. ferritic,
pearlitic, ferrito-pearlitic, martensitic etc.), this grade of S.G.Iron is preferred when these properties become the
prime considerations. In the present work the material’s ability to be used at low (sub-zero) temperatures has been
studied.

* Corresponding author Tel:+91 8309163485

E-mail address: vbrahmi@gmail.com

2214-7853 © 2019 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the 9th International Conference of Materials Processing and Characterization, ICMPC-2019
 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868 4861

1.1 properties to be considered at low temperature

As temperature decreases, the strength of a material increases while ductility and toughness decrease. For a
particular type of materials (mostly the B.C.C materials) there is a temperature range in which there is a sharp fall in
the value of the toughness. So below that temperature region a material which behaves in a ductile manner at higher
temperature becomes brittle. This temperature (actually a range of temperature) at which this transformation takes
place is a called ductile to brittle transition temperature. The F.C.C materials generally do not exhibit any ductile to
brittle transformation as a result of lowering of the temperature. Since S.G.Irons with austenitic matrix possesses
F.C.C structure, they are expected to retain toughness at lower temperatures. But at the same time here the matrix
becomes austenitic only due to addition of suitable alloying elements (in general nickel) so its stability solely
depends on the amount of the austenite stabilizing element(s). So it is to be seen whether toughness can be retained
at subzero temperature. In this work, low Ni S.G.Irons were used to compare their impact properties to the same
properties of austenitic S.G.Iron. In case of low Ni-alloys (which have ferritic/pearlitic matrix) both stress –relieved
annealing and austempered specimens were used. The purpose was to compare the impact properties of all of them
to that of austenitic S.G.Iron.
The morphology and fractrography of Austenitic S.G.Iron or Ductile iron is studied and also several measures
have been taken for the improvement of microstructure. This can be done by adjusting the distribution and
percentage composition of the alloying elements on the alloyed region [3] and [4]. The microstructure of S.G.Iron
exhibits spheroids of graphite in an austenitic matrix. The stabilization of austenitic phase is achieved by
accumulation of elements like Ni, Mg and Cu. If percentage of nickel increases there is an increase in tensile
properties [5]. It has good scaling resistance, high ductility, highest embodied energy, good thermal expansion
characteristics. In addition, it has good corrosion resistance in sea water as well as in alkaline liquids, good cold
toughness and resistance to erosion [6], [7], [8] and [9]. It offers plentiful of economic advantages due to its better
properties than the other grades of ductile iron.

2. Experimental details

2.1 Composition

Two different grades of S.G.Iron were used for the experiment. The first one contained only 0.15% Ni and the
second one contained Ni of significant proportion (12%). So, the first one had a ferrito-pearlitic matrix while the
second one was of austenitic matrix. The details of the composition of both the grades are shown in Table 1.

Table 1. Chemical composition of ductile irons.

Element %C %Si %Mn %S %P %Cr %Ni %Mg %Cu %Fe

0.15 Ni 3.45 2.07 0.15 0.008 0.024 0.02 0.15 0.043 - Rest
DI
Austenitic 3.00 2.42 0.28 0.013 0.030 0.14 12.1 0.066 0.011 Rest
DI

2.2. Heat Treatments

For the S.G.Iron with ferrito-Pearlitic matrix two different types of heat-treatment were performed namely stress
relieving (annealing) and austempering. Stress relieving (annealing) was performed by heating the sample to 600°C,
holding at the temperature for 80 minutes and then cooling it inside the furnace at 285°C and finally to room
temperature. To perform austempering, the specimen was initially heated to 925°C and held there for 80 minutes to
complete austenitizing. Then it was quenched in salt bath (KNO3 and NaNO3) in 1:1 ratio held at 475°C for 41/2 hrs
and finally air cooled to room temperature as shown in below Fig 1 (a-b).
4862 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868

(a) (b)

Fig. 1. Heat treatment schedules (a) Stress relieving (annealing) (b) Austempering process.

The austenitic grade was annealed the sample to 1050°C, holding there for 90 minutes and finally to room
temperature. This heat-treatment schedule has been shown in Fig (2).

Fig. 2. Annealing heat treatment process.

2.3 X-ray Diffraction Analysis

X-ray Diffraction Analysis is performed to detect the phases and study the crystal structure by using X-ray
diffraction analysis. RIGAKU ULTIMA IV diffractometer was used for this purpose (Cu kα target, λ = 0.1542nm).
The scanning rate was 7 °/min in the 2θ range of 20-110° with a step size of 0.02. Here, the crystallographic planes
can be determined from the corresponding peaks. This analysis has been performed by using Xpert highscore along
with JCPDS software. The crystallographic planes pave the way for determination of the crystal structure. It also
helps to determine the amount of retained austenite in austempered ductile iron.

2.4 Optical Microscopy

For the metallographic studies, each sample was mounted and polished with different grades of emery paper and
then cloth polished using alumina. For nodularity and nodule count samples were examined before etching under
optical microscope. 2% nital solution was used as the etchant to develop the microstructures. Microstructures were
observed both before and after heat-treatment.

2.5 Tensile Test

All the heat treated samples were subjected to tensile test. U.T.S. and % of elongation were determined from the
Load vs Displacement plots. The tests were performed with the help of universal testing machine (UTM)
INSTRON-1995. The samples were machined as per ASTM standards [Fig. 3].
 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868 4863

Fig. 3. Specimen dimensions for tensile test according to ASTM standards.

2.6 Impact Test

Impact test was carried out by using Charpy Impact Tester. Samples were V-notched with dimensions 55x10x10
(all in mm) and notch depth 2mm with included angle 45°. Fig. 4 shows the details of the specimen used for impact
testing. The tests were conducted at 20°C and (subzero temperatures) -20°C. The impact tester consists of a hammer
mounted on the handle. A hammer is used to act on the sample in the opposite direction of the notch (which is held
at each end). The energy absorbed upto fracture is the measure of the toughness.

Fig. 4. Shows the specimen dimensions for impact test (all are in mm).

2.7 Fractography

The fractured surfaces (both for impact and tensile tests) were studied under JEOL-JSM6084LY scanning electron
microscope. The purpose of the test was to determine the type of fracture.

3. Results and discussion

3.1 X-Ray Diffraction (XRD) Analysis

The XRD patterns have been shown in (Fig. 5.a) for the Ferrito-Pearlitic ductile iron and in (Fig. 5.b) for the
austenitic ductile iron. B.C.C. structure has been observed in as cast and stress relieved samples. The crystal
structure proves the existence of a ferrite matrix and austempered samples show (110), (211) planes indicating
crystal structures B.C.C. and (200), and (220) as F.C.C. crystal structures, demonstrating the presence of ferrite and
austenite (retained). These volume fractions were calculated by using equations (1 and 2) [10] and [11]. The
calculated ferrite and austenite (retained) values are 80.0% and 20.0% respectively. The presence of carbon in
austenite (retained) is also calculated by using equation (3), it was found to be 1.104%. As can be seen from the
austenitic ductile iron (Fig. 11), all planes are defined as F.C.C. crystal structures, confirming the existence of the
austenite matrix.
4864 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868

I R X 
 ………. (1)
I R R

x  x y  1 ……. (2)

a y  0.3548  0.0044C y ……… (3)

I is Integrated intensity per unit length of diffracted line, R is Theoretical Intensity, X is Volume Fraction, α is
Ferrite, γ is Austenite, is Lattice parameter of austenite peaks, and is Carbon percentage in austenite.Cγ =
Carbon percentage in austenite as shown in below Fig 5 (a-b).

Fig. 5. Shows the XRD peak patterns (a) Ferrito-Pearlitic ductile iron (b) Austenitic ductile iron.

3.2 Morphological studies

The morphological quantification has been shown in Table-2. The graphite area fractions are 16.32%, 16.28% and
6.48% for (as-cast, austempered and annealed) ferrito-pearlitic grade of ductile iron. The matrix becomes bainitic for
the austempered one. The nodule count and nodularity (%) are also shown in the same table. Increase in nodule
count results in enhancement in ductility (% elongation) and reduction in tensile strength. Graphite area fraction is
18% for annealed and 12% for as cast austenitic ductile iron. The microstructures of differently treated S. G. Irons
have been shown in Fig. 6 & Fig. 7 (for ferrito-pearlitic and austenitic grades respectively).

Table 2. Morphological quantification.

Grades Heat Treatment Nodule Count Nodularity (%) Graphite Area

Fraction (%)
Ferritic-Pearlitic As cast 86 98 16.32
Stress relieved 60 83 16.28
Austempered 57 95 6.48
Austenitic As cast 46 96 12
Annealed 36 96 18
 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868 4865

Fig. 6. Microstructures of Ferritic/Pearlitic DI (a) As cast (b) Stress Relieved (c) Austempered.

Fig. 7. Microstructures of Austenitic DI (a) As cast (b) Annealed

3.3 Mechanical Properties

Ultimate Tensile Strength (U.T.S) and Impact toughness have been determined for all the specimens.
3.3.1 Tensile Strength
The results have been shown in Table-3. From the results we see that the austempered specimen has got higher
tensile strength than the other ones of the ferrite-pearlitic grade while the austempered samples have got the lowest
ductility (as evidenced by the % of elongation). The elongation is minimum for the austempered specimen (10.33%)
Table 3. Results of tensile test.

Sample U.T.S (Mpa) % elongation

Ferritic/pearlitic DI As cast 342.0 19
Stress relieved 331.16 23
Austempered 727.4 10.33
Austenitic DI As cast 310 23.00
Annealed 290 26.00

due to the presence of hard upper bainitic matrix. The % of elongation for as cast and stress relieved specimens has
been found to be 19% & 23% respectively. The strength decreases and ductility (% of elongation) increases for the
austenitic matrix. The annealed austenitic ductile iron specimen exhibits 26% of elongation as shown in above fig6
(a-c) and Fig 7 (a-b).
4866 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868

3.3.2 Impact Toughness

The results of the impact tests have been shown in Table-4. The tests were performed at 20°C and -20°C for both
the ferrito-pearlitic and austenitic grades. The results show that there is significant drop in the value of impact
energy with the lowering of temperature for the ferrito-pearlitic grade but the austenitic grade retains the same value
even at a temperature as low as -20°C.
Table 4. Results of impact test.

Ferritic/pearlitic DI Sample Impact energy (J)

Room temp -20°C
As cast 16 14
Stress relieved 18 17
Austempered 14 10
Austenitic DI As cast 16 16
Annealed 19 19

3.4 Fractographic study

The fractured surfaces of the broken samples (of both impact and tensile tests) were viewed under the scanning
electron microscope (S.E.M) to study the different features revealed by the fractographs.

3.4.1 Impact Specimens

3.4.1.1 Fractographs of impact specimens tested at room temperature

The fractographs shown in Fig. 8 (a-c)and Fig. 9 (a-b) reveal the different features of the impact specimens tested
at 20°C. While Fig. 10 (a-b) and Fig. 11 (a-b) show the same for the specimens tested at -20°C. The mode of failure
in almost all the specimens are mostly ductile only the austempered ferrito-pearlitic specimens contain some
evidence of brittle fracture as evidenced by the presence of river markings which are more vivid in the austempered
specimens tested at -20°C (Fig. 10.c)

Fig. 8. Microstructure at room temperature (a) As cast (b) stress relieved (c) Austempered Ferritic/ Pearlitic Ductile iron
 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868 4867

Fig. 9. Microstructure at room temperature (a) As cast (b) Annealed Austenitic Ductile Iron

Fig. 10. Microstructures at -20˚C (a) As cast (b) stress relieved (c) Austempered Ferritic/Pearlitic Ductile iron

Fig. 11. Microstructures at -20˚C (a) As cast (b) Annealed Austenitic Ductile Iron

4. Conclusion

By analyzing the results it can be concluded beyond doubt that ductility and toughness increases for ductile iron
with the addition of nickel which results in an austenitic matrix.
 The most important observation is that there is no decrease in the value of impact energy for the austenitic
ductile iron with the fall in temperature.
 It must be noted that in this experiment we have used austenitic grade of ductile iron containing just 12%
Ni and still the room temperature toughness (which is evidenced by impact energy) is retained even at -
20°C.
 So it may be concluded that with higher Ni content in the austenitic grade of ductile iron, the toughness can
be retained even at lower temperatures.
 So it is quite reasonable to draw the inference that austenitic ductile iron is worthy of being used as a low
temperature material.
4868 S. Shama et al./ Materials Today: Proceedings 18 (2019) 4860–4868

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