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The Effect of Inoculation on Microstructure and Mechanical Properties of

Ductile Iron

Article · January 2013

DOI: 10.9790/1684-0561723

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Bahubali Sangame
Sharad Institute of Technology College of Engineering, Yadrav Ichalkaranji
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IOSR Journal of Mechanical and Civil Engineering (IOSR-JMCE)
e-ISSN: 2278-1684 Volume 5, Issue 6 (Mar. - Apr. 2013), PP 17-23
www.iosrjournals.org

The Effect of Inoculation on Microstructure and Mechanical

Properties of Ductile Iron
Mr. Bahubali B. Sangame1, Mr. Vasudev D. Shinde2
1
(P. G. student at D.K.T.E.’s Textile and Engineering Institute, Ichalkaranji, 416115, India.)
2
(Associate professor at D.K.T.E.’s Textile and Engineering Institute, Ichalkaranji, 416115, India.)

Abstract: The current work proposes thermal analysis system for analysis of ductile iron solidification
processing. The system consists of standard pouring cup with built in thermocouple. The thermocouple is
connected to data logger system so as to store temperature data of solidification sequence. The ductile iron
treatment consists of composition control, melt pre-treatment, magnesium treatment and inoculation processing.
Even small change in processing can be monitored by thermal analysis and its effects on final microstructure
and mechanical properties were studied. Along with test cups, the tensile test bars were also poured and
analyzed for correlating the mechanical properties with solidification sequencing. The melting trials with
varying amount of inoculation processing were conducted to study its effect especially on amount of nodule
count, nodularity and amount of pearlite and ferrite phase. As the microstructure decides the final mechanical
properties in ductile iron castings, the nucleation and proportion of these phases is of paramount importance
during solidification. The thermal analysis of base metal and inoculated material can be effectively used for
improving mechanical properties of ductile iron castings.

I. Introduction
Many of the steel components are replaced by ductile iron due to high strength to weight ratio and
range of properties. The ductile iron provides good combination of strengths and ductility due to presence of
spheroidal graphite. From a metallurgical view, ductile iron is one of the most complicated materials. During
solidification several phases were nucleating and interaction of these different phases during growth is very
complicated. The occurrence and distribution of these phases have major impact on the final mechanical
properties of the casting. It is therefore interesting to understand how the different phases nucleate and grow
during solidification in order to be able to control the casting process and achieve the right mechanical
properties [1].
The commonly used mechanical properties for ductile iron are tensile strength, yield strength, percent
elongation and brinell hardness. Because of the nominal and consistent influence of spheroidal graphite, the
tensile properties and the brinell hardness of ductile iron are well related. The relation between tensile properties
and hardness depends on structure of its base matrix. In the matrix, the softer ferrite gives higher ductility but
lower yield strength than pearlite. Also the graphite morphology plays an important role and the more the
graphite shape deviates from the ideal spherical shape, the lower is the ductility and strength [2]. The time after
spheroidal treatment has significant effect on the elongation, but insignificant effect on the tensile strength and
hardness of castings. Even small changes of the elements show significant increase or decrease in mechanical
properties of ductile iron [3].
The chemical composition, melt treatment and cooling rate are important processing parameters which
decide the final properties of ductile iron. The graphite nodule count and nodularity (deviation from spherical
shape) and the amount of phases are to be controlled to achieve better combination of properties in ductile iron.
Melt treatment consisting of modification and inoculation, in which initially magnesium treatment of the melt is
done (for changing graphite shape from flake to spheroidal) and further inoculation (for increasing the nodule
count or to suppress carbide formation) is must [4]. In case of hypoeutectic ductile iron,solidification proceeds
by nucleation of austenite, and graphite spheroids nucleate on pre-existing austenite and grow in the
interdendritic regions. In hyper eutectic melts, solidification starts with graphite nodules [5,6], which reduces
the remaining carbon in the liquid, upon further cooling, the austenite grows dendritically and thus allowing new
graphite spheroids in interdendritic regions[7]. Graphite nodules nucleate on small inclusions [8] but further
growth solely depends on foreign particles or solutes which are added as inoculant [5].
Rare earth elements reduce the magnesium requirement for a particular set of nodule count and
nodularity. As some of the magnesium measured is in the form of magnesium sulfide, final iron sulfur level
affects the magnesium needed to result in nodular graphite. Maximum nodularity can be achieved by keeping
magnesium residual just enough (0.02%) will deteriorate the nodule shape from fully spheroicity [9]. Nodule
count can be maximized by sound base iron melting practice and good inoculation practice. Nodule count and
nodularity is affected by cooling rate. Thin section regions due to fast cooling results in better nodule shape than

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 The Effect of Inoculation on Microstructure and Mechanical Properties of Ductile Iron

slowly cooled ductile iron for the same magnesium residuals. Larger sections require increased magnesium
residual whereas late inoculation reduces the magnesium requirement[10]. In conjunction with this, current
research work attempts to establish relationship between chemical composition, inoculation processing and
pouring temperature of casting by solidification thermal analysis and comparing with experiments.

II. Experimental Procedure

To study the solidification process and its effect on mechanical properties, one needs to study heat
transfer analysis of solidification sequences in ductile iron. The current study comprises of capturing
solidification temperature data by built in thermocouples fitted in cup casting. Measuring and correlating the
properties in castings by analyzing cooling curves. The cup is made up of shell sand, with 21x21x42mm cavity
(Electronite standard QC-4010) as shown in Fig.1. The weight of cup casting is 0.315 kg having modulus
(volume/ surface area) of 7 mm.
The melt charge consisting of 15-20% pig iron, 30-35% Cold rolled steel scrap and remaining foundry
returns is melted in 500 kg capacity coreless medium frequency induction furnace. The raw materials are tested
for its chemical compositions by spectrometer analysis and are reported in Table 1.The molten metal was tapped
in a preheated ladle containing Ferro-silicon-magnesium alloy of size 10-15mm at the bottom covered with steel
scrap. The tapping temperature of molten metal was 1450oC.The inoculant is then added in the melt, while
pouring directly in the stream for proper mixing (Fig.2 a). Inoculant of size 2 to 4 mm is added in molten metal
stream so as to dissolve easily and should be dust free to avoid losses due to oxidation or thermal air currents.
Total four ductile iron melts were poured using transfer ladle treatment method as shown in Table 2.

Table 1: Details of furnace charge mix along with spectroscopic analysis

Charge Amount Size/shape Mg Ca Al Ba
materials C Si Mn P S
Pig iron 65 kg Briquettes 4.13 1.91 0.14 0.075 0.025 -- -- -- --
Foundry 135 kg Gating 3.68 2.21 0.18 0.010 0.026 -- -- -- --
returns
Steel scrap 300 kg Punching 0.038 0.001 0.302 0.025 0.008 -- -- 0.04 --
Fe-Si-Mg 1.8 kg/150 10-15 mm -- 47.50 -- -- -- 5.82 1.23 0.92 --
alloy kg ladle
Inoculant 200gm/50Kg 2-4 mm -- 74.62 -- 0.035 0.004 -- 1.13 1.41 2.47

(a)

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 The Effect of Inoculation on Microstructure and Mechanical Properties of Ductile Iron

Fig.1: a) Ductile iron Non-Tellurium cup with standard Electronite-QC-4010, Cup stand b) poured cup and c)
die assembly for sampling of chemical analysis test

Fig.2: a) Stream inoculation process, b) Data acquisition system comprising of DAQ, thermocouples and
pouring cup
While pouring, sample was taken from the melt for spectroscopic analysis. The treated iron was poured into
shell molds for tensile test sample and cup castings for thermal analysis (Fig. 3). The pouring temperature
recorded is 1380oC. Similarly remaining melts were properly inoculated with each melt having varying amount
of inoculant. In the varied inoculation trials, three cups were arranged in such a manner that pouring will be
done in a sequential manner. K type thermocouples connected to each cup casting to capture temperature during
solidification. ADAQ-3005 (MCC-USA) data logger for data acquisition synchronized with Desylab 12.0
software for analysis(Fig.2 b).Temperature time data thus captured can be further processed to plot cooling
curves of individual melts processed differently. Metal samples are taken for spectroscopic analysis while
pouring so as to measure final chemistry of the castings being poured. The final chemistry for each melt was
determined using Spectrometer (Spectro-lab, M-9 model, German make). These chilled specimens were grinded
on sand paper for performing the chemical analysis (Table 2).

Table 2: Chemical analysis of 0.4%, 0.6% and 0.8% Inoculated metal.

% % % % % % % % % % %
Metal Treatment
C Si Mn P S Cu Al Ca B Ce Mg
Base Metal 3.64 1.2 0.183 0.034 0.011 0.099 0.009 0.001 0.001 0.005 0.005
A) 0.4% Inoculation 3.65 2.3 0.159 0.028 0.012 0.10 0.023 0.001 0.001 0.011 0.035
B) 0.6% Inoculation 3.65 2.5 0.173 0.032 0.012 0.12 0.03 0.002 0.003 0.01 0.039
C) 0.8% Inoculation 3.63 2.6 0.187 0.031 0.007 0.11 0.023 0.001 0.002 0.016 0.042

III. Results
The experiments are conducted in ductile iron jobbing foundry and the results of thermal analysis,
microstructural analysis and mechanical properties are presented as follows:

3.1: Thermal Analysis

The magnesium treatment is performed by transfer ladle process into 150 kg ladle. The base metal
sample is taken after completion of charging and melting and poured into cup for thermal analysis as shown in
Fig. 3 (a). The Mg treated metal is transferred into ladles of 50 kg and inoculated with A) 0.4% with 0.2kgof
inoculant, B) 0.6% with 0.3kgof inoculant and C) 0.8% with 0.4kgof inoculant respectively (Table 2). The
thermal analysis of metals with different inoculant is shown in Fig. 3(b).The thermocouples inserted in each cup
casting records the thermal history of solidification process.
In the current experiments, the cooling curves are generated from solidification temperature history of
solidifying base metal cup.It is observed that lower eutectic undercooled temperature(TEU)for base metal is 1119
o
C and TER temperature is 1132 o C which shows the larger undercooling effect which gives larger recalescence
degree. The cooling curves generated from 0.4%, 0.6% and 0.8% inoculated cups, indicating the decreasing
amount of recalescence as shown in Fig. 4(b). Larger the undercooling, more are chances of formation of
undesirable carbides. The minute details of undercooling, recalescence and total solidification time values are
used to correlate these solidifying details with final microstructure and mechanical properties.

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 The Effect of Inoculation on Microstructure and Mechanical Properties of Ductile Iron

(a)

ΔT
ΔTRR

(b)

Fig.3:Cooling curve for a)base metal, b) Ductile iron with varying amount of inoculant
In the cooling curve (Fig. 3)TM - Maximum temperature of the melt (oC); TGL - temperature of graphitic
liquidus (oC); TEU-Temperature of eutectic undercooling (oC); TER - Temperature of the graphitic
recalescence(oC); ΔTR- Recalescence (oC); TES - Temperature at the end of solidification (oC);tS-Total
solidification time (sec).When the liquidus temperature (TGL) is reached, the cooling curve shows a quasi-
horizontal plateau. This point means that, the heat losses are exactly balanced by the amount of heat of
solidification. The length of the horizontal plateau is the total solidification time needed for the graphite to grow.
However, the decrease of temperature continues till the lowest eutectic temperature (TEU). The solidification
cooling curve normally shows undercooling at start of solidification. This undercooling is the driving force for
nucleation. The period of nucleation isnormally short and is followed by an increase in the temperature giving a
maximum temperature (TER) shortly after the nucleation event. At eutectic temperature, simultaneously austenite
and graphite gets precipitated from the liquid melt. After TEU, the solidifying metal releases heat which shows
overall increase in temperature, is referred as recalescence (ΔTR) which is measure of difference between (TER)
and (TEU).

Table 3: Critical temperatures derived from thermal analysis

Temperature (oC)
Specific Temperature
Base metal A 0.4 % B 0.6 % C 0.8 %
(uninoculated) Inoculant Inoculant Inoculant
Lower eutectic temperature(TEU) 1119 1140 1141 1145.5
Eutectic Recalescence temp.(TER) 1132 1145 1144 1148
ΔTEU= TEU (Ino.) – TEU (Unino.) --- 21 22 26.5
ΔTR= TER – TEU 13 5 3 2.5

The ΔTEU is the difference in temperature of eutectic undercooling of inoculated and uninoculated iron and
reported in Table 3. Also the recalescence is a measure of difference in T ER and TEU (ΔTR = TER – TEU), Where
tSA, tSB and tSC are the eutectic solidification times for 0.4%, 0.6%, 0.8% inoculated metals in seconds. In the
current experimental conditions, the difference between the TEU temperatures of inoculated and uninoculated
iron (ΔTEU) was observed in the range of 21-26.5 oC. A higher TEU value indicates that metal is more resistant to
chill than with a lower TEU value. The highest eutectic temperature (TER) is attained as a result of increase in
temperature because of the release of inherent heat called latent heat. The recalescence (ΔT R = TER- TEU) reflects
the amounts of austenite and graphite that precipitate during the first part of eutectic freezing. Too high
recalescence might be harmful especially in soft moulds, as the volume expansion is high and might increase the
size of the mould cavity. The ideal recalescence depends on casting material and its modulus. In well inoculated
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 The Effect of Inoculation on Microstructure and Mechanical Properties of Ductile Iron

ductile iron casting, less than 5oCrecalescence is preferred. Lower level of recalescence will depict high
efficiency of inoculants and the risk for micro shrinkage and porosity will be reduced.

(a) (b)
ΔTEU

ΔTR
Fig. 4:a) Undercooling difference between inoculated and un-inoculated ductile irons b) Recalescence degree of
inoculated ductile iron

3.2: Microstructure analysis

The samples for microstructural observation were taken from the center of the casting and polished
properly. The samples were etched with 2% Nital (2% concentric Nitric acid and 98 ml Methylalcohol). Then
optical micrographs were taken with a 35 mm camera attached to a Leintz microscope.

Table 4: Analysis of microstructure in inoculation varied ductile iron samples

Inoculation amount % Nodularity Nodule count(/mm2) % Ferrite
0.4% 84 205 88.43
0.6% 90 264 90.24
0.8% 95 291 94.09

The polished samples after metallographic analysis were put under Image Analyzer (Make-ProMetal-11) to
investigate the nodule count, nodularity and percentage of ferrite and pearlite content in the cast samples (Fig. 5).
A microstructure analysis result of 0.4, 0.6 and 0.8% inoculated metal showing increase in nodule count,
nodularity and ferrite % with amount of inoculation (Fig. 6). The nodule count increases from 205 to 291, %
nodularity from 84 to 95 and % ferrite from 88 to 94 % with increase in inoculation from 0.4 to 0.8 %
respectively (Table 4).

Fig.5:Microphotographs of ductile iron samplesindicatingunetched (A, B and C) and etched with Nital(A-E, B-
EandC-E)inoculated with 0.4 %, 0.6% and 0.8% respectively

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 The Effect of Inoculation on Microstructure and Mechanical Properties of Ductile Iron

(a) (b)

Fig. 6:a) Effect of % inoculation on nodule count. b): Effect of % inoculation on % elongation.

3.3: Mechanical properties

The ductile iron inoculated metal in also poured into the shell mould of tensile bar as shown in Fig. 7
(a) so as to prepare tensile sample as per ASTM E-24 standard Fig.7 (b). After machining of tensile cast bars,
these samples are tested for tensile strength and results are reported in Table 5. The thermocouples inserted in
each cup casting records the thermal history of solidification process. From each melt the tensile bars are poured
and machined to prepare specimens for conducting tensile test as per ASTM standard E-24. The tensile strength
and elongations results measured using MTS machine were reported in Table 5. The tensile strength decrease
from 483 to 421 MPa with increase in elongation from 15.7 to 21 % with increase in addition of inoculant from
0.4 t o0.8 % respectively.
(b)

Ø12

Ø20

50

20 57 20

112

Fig. 7: (a) Test bar mould poured with molten metal, and b) Specifications of tensile specimen as per ASTM E-
24
Table 5: Effect of inoculation variation on tensile strength of ductile iron
Inoculation amount % Elongation Tensile strength (Mpa)
0.40% 15.73 482.95
0.60% 18.21 452.74
0.80% 21.1 420.85

IV. Discussion
Experiments have been performed on ductile iron melts with base metal composition and inoculated
metal with varying amount of inoculants. The thermal history of solidification processing is being recorded
which will be used to correlate microstructural evolution of the solidified structures and mechanical property
measurements. In case of un-inoculated (base) metal, the recalescence (ΔTr) is 13 oC, which indicates need of
larger driving force for the solidification process. However, the higher undercooling before recalescence
increases the risk of formation of carbides in the solidified structure. In case of inoculated metal, the
recalescence value is within 5 oC. The increase in amount of inoculation shows decrease in recalescence value.
The basic function of inoculation is to increase nucleation sites, thereby reducing undercooling and promoting
the graphite nucleation which minimizes the risk of formation of hard eutectic carbides. The cooling curves of
inoculated metal reveal that, the eutectic undercooling temperature (TEU) increases with increase in inoculation.

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 The Effect of Inoculation on Microstructure and Mechanical Properties of Ductile Iron

The solidification times of melts A to C (tSA, tSB, and tSC) increases with increased amount of inoculant addition.
Nodule count, expressed as the number of graphite nodules/mm 2, also influences the mechanical properties of
ductile iron, although not as strongly and directly as graphite shape. Generally, high nodule count indicates good
metallurgical quality, but there is an optimum range of nodule count for each section size of castings, and
nodule count in excess of this range may result in a degradation of properties. Thermal analysis cups are
designed such that, it weighs 315 gms having modulus of 7mm, offers cooling rates such that it gives optimum
combination of tensile strength and ductility, which is followed as guideline for making casting of nearby
modulus.

V. Conclusion
The experiments were conducted on ductile iron with varying amount of inoculant. The cup thermal
analysis can be effectively used for measuring performance of amount of inoculant on solidification of ductile
iron castings. Within the experiments conducted, the following conclusions were highlighted:
 Nodule count influences the pearlitic content of as-cast ductile iron. Increasing the nodule count decreases
the pearlite content and tensile strength and increase in % elongation.
 Increasing the nodule count improves ductility which reduces the tendency of formation of chill carbides.
 Matrix consistency is influenced by nodule count. Increasing the nodule count produces a finer and more
homogeneous microstructure. This refinement of the matrix structure reduces the segregation intercellular
harmful carbides, pearlite or degenerated graphite.
 Inoculation practices used to improve nodule count often make the nodules more spherical. Thus, high
nodule count is generally associated with improved nodularity offering increase in toughness.
 The increase in amount of inoculation decreases the recalescence and amount of undercooling improving
overall properties of ductile iron.

Acknowledgement
Author gratefully acknowledges the assistance of S. S. Industries,Ganeshnagar,Ichalkaranji for
supporting melting trials, thermal analysis and microstructure analysis and M/s Suyash enterprises, Pune for
supporting thermal analysis for providing thermal analysis cups.

References
[1]. O. SeiduS., I. Riposan, “Thermal analysis of inoculated ductile irons”, U.P.B. Sci. Bull., Series B, 73(2), (2011) pp. 241-253.
[2]. D. Sparkman, “Using thermal analysis practically in iron casting,” Modern casting. (1994).
[3]. S. Bockus, A. Dobrovolskis “Peculiarity of Producing Ferritic Ductile Iron Castings”, Materials Science (Medziagotyra), 10, 1, (2004)
pp. 3-6.
[4]. Rio Tinto Iron and Titanium, “Ductile Iron Databook for Design Engineers”, Monreal, (1999), pp. 250.
[5]. J. Campbell in Castings Principles, the “New Metallurgy of Cast Metals Elsevier”, Amsterdam. (2004).
[6]. M. C. Flemings, in “Solidification Processing”, McGraw-Hill Book Company, New York, (1974) pp. 423.
[7]. T. Skaland, in proceedings of the AFS cast iron, schaumburg, Illinois, (2005) pp. 29-30.
[8]. G.L. Rivera, R.E. Boeri, and J.A. Sikora, AFS Transactions, (2003) pp. 111, 979.
[9]. J.D. Mullins, in manual of Sorelmetal, Technical services, Rio Tinto Iron and Titanium, (2006).
[10]. T. Skaland, Ø. Grong and, T. Grong, “Metallurgical and Materials Transactions” A, 24(A), (1993), pp. 2321.

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