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Formation of microstructures in the spheroidal graphite cast iron

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2012 IOP Conf. Ser.: Mater. Sci. Eng. 27 012064
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The 3rd International Conference on Advances in Solidification Processes

IOP Publishing
IOP Conf. Series: Materials Science and Engineering 27 (2011) 012064
doi:10.1088/1757-899X/27/1/012064

Formation of microstructures in the spheroidal graphite cast

iron
S. Wang1, D. Daloz1, F. Bruneseaux2 and G. Lesoult1
1
IJL-SI2M, UMR7198-CNRS, Nancy-Universit, UPV-Metz, Ecole des Mines de
Nancy, Parc de Saurupt, CS 14234, F-54502 NANCY, Cedex, France
2
Centre de Recherche et Dveloppement de St Gobain, Maidires-ls-Pont-Mousson, 54704 PONT-A-MOUSSON, Cedex, France
E-mail: dominique.daloz@mines.inpl-nancy.fr
Abstract. Pipeline systems for hydraulic networks are obtained via centrifugal casting of
spheroidal graphite cast iron. The very high cooling rate that is achieved in the skin of the
product can sometimes lead to carbide instead of graphite in cast iron. An experimental device
has been built in the laboratory that allows reproducing the extreme thermal conditions
encountered during formation of skin of centrifugally cast pipes. Liquid metal droplets fall on a
cold substrate. Rapid directional solidification occurs. The temperature evolution of the lower
surface of the droplet is recorded during the very first moment of the solidification (t < 200 ms)
thanks to a photodiode, which is located below the substrate. The microstructures that are
obtained in laboratory are characterised in both the as-cast state and the heat-treated state. They
are compared to the centrifugally cast ones. A model of directional solidification of cast iron
under a very large temperature gradient has been built. It allows explaining the transition from
stable to metastable microstructure that was observed in the products and reproduced in the
laboratory samples.

1. Introduction
The thermal conditions and the treatment of the liquid metal for centrifugal casting of pipes lead to the
solidification of the melt in the form of spheroidal graphite (SG) iron throughout the thickness.
However, sometimes there are zones to be observed that are solidified within the white mode (eutectic
austenite / cementite) mainly in the skin of the product. These areas lead to differences in the
metallurgical response, which are problematic during the subsequent heat treatment.
The obtention of SG iron is controlled by the preparation of the liquid metal (magnesium treatment
+ inoculation treatment) and by the cooling mode. Under moderate cooling conditions, the influence
and effectiveness of these treatments is known and various models are available in the literature to
describe the solidification [1]. When the cooling rate increases as in the first skin of centrifugally cast
pipe, one can observe a microstructural transition leading to the formation of white iron. This
transition is traditionally explained in terms of maximum undercooling achieved for the nucleation of
the cementite (competition of nucleation) and / or a growth competition between graphite and
cementite. While the transition is well documented in the literature [2-7], most of the articles deal with
the influence of cooling rate as the natural variable controlling the transition. This variable, of
common practice does not satisfactorily account for describing into details the origin of the

Published under licence by IOP Publishing Ltd

The 3rd International Conference on Advances in Solidification Processes

IOP Publishing
IOP Conf. Series: Materials Science and Engineering 27 (2011) 012064
doi:10.1088/1757-899X/27/1/012064

microstructures for a given composition: for this it is necessary to decompose the cooling rate in terms
of the product of thermal gradient and solidification rate.
The aim of this study is to characterise and understand the mechanisms responsible for the formation
of the structure in the first skin of the centrifugal casting of SG iron. We describe in this article the
experimental technique developed in order to capture the phenomena linked to the very beginning of
solidification. We present the experimental results and the basis of a solidification model developed in
order to interpret the results.
2. Experimental Technique
2.1. Falling droplet experiment.
The falling droplet experiment allows the study of the first moments of the solidification of an alloy
cast onto a metallic substrate that is instrumented and representative of the centrifugal die [8]. Its
principle is to project a small mass of liquid iron, between 5 and 7 g on a substrate cooled by water
circulation. The surface temperature of the melt that solidifies in contact with the substrate is measured
using a silicon photodiode. The optical sight of the metal surface is carried out through a hole 0.3 mm
in diameter drilled in the substrate. The main advantage of the device is its high acquisition speed
(between 2.5 and 10 kHz) and its low dead time (less than 300 s), allowing accurate monitoring of
changes in cooling conditions in solidification. A schematic of the experimental device used and
developed in the laboratory is shown in figure 1.

Figure 1. Falling droplet experiment

2.2. Metal preparation

Industrially obtained spheroidal graphite cast iron in centrifugal casting as a part requires processing
of liquid metal by adding magnesium just before pouring it together with inoculation of molten metal
during casting by adding an inoculants onto the surface of the centrifugal shell. The device developed
in the laboratory does not allow, in a reproducible way, to add the magnesium in the liquid metal just
before it is ejected. To overcome this obstacle it was decided to overdose magnesium in the mother
alloy. To determine the operating conditions similar to industrial conditions we determined the loss of
magnesium associated with the superheat temperature above the liquidus and the holding time
corresponding to this temperature. All the tests presented below were made from an hypereutectic cast
iron of composition Fe-3,9%C-2.37%Si- 0.096%Mg (wt%). The overheating of the drop before
ejection was set to 50 C for a time of 30s leading to a residual Mg content of 0.06% which is
representative of industrial conditions. Inoculation of the cast iron was realised by addition of
Spherix in the same manner as the industrial practice.

The 3rd International Conference on Advances in Solidification Processes

IOP Publishing
IOP Conf. Series: Materials Science and Engineering 27 (2011) 012064
doi:10.1088/1757-899X/27/1/012064

2.3. Metallographic preparation

The samples were characterised metallographically by optical microscopy and scanning electron
microscopy. The samples were cut, coated, and polished mechanically to finish with a diamond
suspension particle (0.5 microns). The determination of the density of graphite nodules and the volume
fraction of graphite was performed by image analysis. Each data represents the average of
measurements on three different fields. A heat treatment similar to the industrial processing was
performed on the as cast droplet.
3. Experimental results
The evolution of the microstructure solidified from the substrate in the case of droplet or shell in the
case of cast pipe after the heat treatment is shown in figure 2. The volume fraction of the graphite
measured on the surface is plotted parallel. One can noticed that, after the heat treatment, the
microstructures are similar in terms of spatial distribution (density of nodules) as well as the volume
fraction of graphite. The volume fraction of graphite being in the range of 11% corresponds to the
equilibrium volume fraction and is constant along the thickness. Figure 3 shows the microstructure of
a centrifugally cast pipe in the as cast state (before heat treatment) and in the case of a droplet. The
evolution of the volume fraction of graphite is reported vis--vis along the distance to the surface
(product thickness). On the surface of the droplet carbides (metastable eutectic) are found. In both
cases one observes an increase in the density of nodules along the thickness of the product correlated
with changes in the volume fraction of graphite measured: 4 to 10% in the case of the pipe and 0,2 3% in the case of droplet.
3.1. Structural evolution of the centrifugally cast pipe.
In the as cast state the volume fraction of graphite along the product thickness increases form 4 to
10%. During the heat treatment, the volume fraction of graphite increases and becomes homogeneous
along the thickness to a value of 11% and a constant density nodule (not reported in this study). The
value of 11% after heat treatment is closer to 10% measured in the as cast state to 3 mm from the
surface. The small difference reflects the fact that at this point the as cast pipe structure is already
practically the equilibrium one.
3.2. Structural evolution of the droplet
In the case of droplets one observes an area virtually devoid of graphite nodule with a thickness of
about 200 m, with a volume fraction of graphite measured in the range of 0.2%. Although initially
greatly different, during the heat treatment the microstructure of droplets evolve similarly to that of the
centrifugally cast pipe in terms of density and in volume fraction of graphite nodule: the as cast
structure of solidification of the droplet can be considered as a precursor of the cast pipe
microstructure. In that way these observations indicate the development of first skin microstructure of
centrifugally cast pipe.
The microstructural evolution during similar heat treatment indicates the presence and efficiency of
nucleation sites of graphite in the droplet from the first moment of solidification. In the case of the
pipe, these sites are also present but one can suppose that in this case, the thermal inertia of the
product produced a first heat treatment in the as cast state leading to the difference in graphite volume
fraction measured between the two as cast states.
4. Physical modelling
4.1. Description of the model
The observation of the microstructure shows that even under very high thermal gradient the
competition between the nucleation of the stable eutectic (graphite + austenite) and the growth of the
metastable one occurs since the very beginning of solidification. To take this competition into account
we built a simple physical model assuming that all the heat transfer proceeds by conduction within the

The 3rd International Conference on Advances in Solidification Processes

IOP Publishing
IOP Conf. Series: Materials Science and Engineering 27 (2011) 012064
doi:10.1088/1757-899X/27/1/012064

substrate and solidification taking place directionally (1D modeling). A front tracking method is used
based on [9] from which the position of the interface and the temperature profile within the droplet is
determined at each time step.

Surface
(Substrate)

Surface
(shell)

Figure 2. Micrograph and volume fraction of graphite nodules measured in the heat-treated state in the
case of a droplet or a pipe. The bottom of the photograph corresponds to the chilling surface.

Surface
(substrate)

Surface
(Shell)

Figure 3. Micrograph and volume fraction of graphite measured in the as cast state in the case of a
droplet or a pipe. The bottom of the photograph corresponds to the chilling surface.
The heat equation is solved with finite difference method using an implicit scheme. A constant
temperature at the outer surface of the product and a constant cooling rate at the liquid/substrate
interface gives the boundary conditions. The following hypotheses/conditions has been used:
i)
graphite nodules nucleate and grow since the liquid temperature fall below the graphite
liquidus. For the sake of simplicity no thermal or chemical effect are taken into account
associated with the growth of the nodule. The following equations (1-2) [3] are used to
determine the nodule density.
g n 1
L

dN = An (T )
dN = 2

d(TLg )
dt
dt

d *TLg +
>2
dt
d *TLg +
<2
dt

if

if

(1)
(2)

The 3rd International Conference on Advances in Solidification Processes

IOP Publishing
IOP Conf. Series: Materials Science and Engineering 27 (2011) 012064
doi:10.1088/1757-899X/27/1/012064

With N the number of graphite nodules at the time t. An and n, constant of the germination
g
law and TL the local undercooling of the liquid relative to the graphite liquidus.

ii)

The carbide/austenite eutectic grows once the liquid temperature fall below the metastable
eutectic temperature, entrapping the graphite nodules. The relation between the interface
temperature and the growth rate is determined from the equation (3) [3] :

vs =

*TEm +4
6 K I K D

(3)

With TEm the growth undercooling, K I a capillarity term and K D a solutal term. The
interlamellar spacing dL of the eutectic is then determined from (4):

K I
dL =
K D vs

(4)

In front of the metastable eutectic, graphite nodules nucleates and grow continuously before being
captured, their density and size being controlled by the local undercooling determined by the thermal
gradient in front of the metastable eutectic front.
4.2. Results
Figure 4 shows the calculated evolution of the temperature in the droplet as a function of its thickness
for a cooling rate of 350 K/s. We also state in this figure the graphite liquidus temperature (1513 K)
and the metastable eutectic temperature (1384 K). One observes along the thickness the decrease in the
growth undercooling of the metastable eutectic. This leads to a decrease in the solidification rate that
consequently increase the time for the graphite nodules to nucleate and grow. In the figure 5 the
calculated interlamellar spacing is shown together with the experimental measurements on the droplet
and on the as cast pipe. One observes the increase of the calculated lamellar spacing with the solidified
thickness in agreement with the decrease of the growth undercooling. The experimental data show a
rather good correlation with the calculated data at the very beginning. Once 100 m are solidified, the
measured interlamellar spacing is higher than the predicted one, those concerning the droplets being
smaller than the one concerning the as cast pipe.
1600
1550

TLiquidus Graphite

Temperature (K)

1500
1450

TE metastable

1400
1350

5 ms
20 ms
80 ms
300 ms
T*

1300
1250
1200
0

500

1000

1500

2000

2500

3000

3500

4000

distance to the surface (m)

Figure 4. Temperature evolution as a function of

the distance to the surface

Figure 5. Lamellar spacing as a function of the

distance to the surface.

The difference between measurements and calculated data indicates a decrease in the heat extraction
rate while solidification proceeds, greater in the case of the as cast pipe than in the case of the droplet.
This could be attributed to an increase of the heat transfer resistance that may be due to an air gap
formation once a certain amount of the skin is formed, or/and a decrease of the radiative transfer
5

The 3rd International Conference on Advances in Solidification Processes

IOP Publishing
IOP Conf. Series: Materials Science and Engineering 27 (2011) 012064
doi:10.1088/1757-899X/27/1/012064

(which is not taken into account in the model) or to an extra reheating by hot liquid in the case of the
as cast pipe (which is much larger than the droplet).
Concerning the nodules density, preliminary results indicates a good agreement with the measured
density, provided that the An term of the nucleation law (equation (1)) is fixed to An = 4000.
5. Conclusions
The aim of this work is to get a deeper understanding on the structure formation of the nodular cast
iron at the first instant of solidification. An experimental setup has been built together with a simple
physical model. We have shown that:
- the falling droplet technique was able to froze the solidified microstructure in an earlier stage
of formation than observed in the as cast pipe. Since the very first moment, graphite
nodules are already present even in the skin of the product. Due to their small size they
represent a low volume fraction (<0,2%) in the droplet and (4%) in the as cast pipe.
- The physical model allows determining the thermal evolution during solidification, the
interface temperature, velocity and structural parameters like the lamellar spacing.
- A good agreement between the experimental measurement and the lamellar spacing is
observed in the very beginning of solidification. While solidification proceeds, the
difference between measurements and calculated data increases. We suggest that this is
correlated to a combination of an air gap formation/ radiative effect. A further difference
exist between the droplet and the as cast pipe that leads to larger lamellar spacing in the
as cast pipe. This may be correlated to the in situ heat treatment leading to the higher
volume fraction of graphite measured in the as cast pipe.
A good agreement is obtained concerning the experimental measurement of the nodule density and the
calculated one, provided the nucleation law parameters are fixed to a rather high value.
References
[1]
Lesoult G - Trait des matriaux 5 : Thermodynamique des matriaux - Presses
polytechniques et universit romandes 2010, ISBN 978-2-88074-690-2, 873
[2]
Lacaze J, Castro M, Aichoun N, Lesoult G 1989 - Revue de Mtallurgie 2 81
[3]
Lacaze J, Castro M, Lesoult G 1998 Acta Metallurgica 46 997
[4]
Lesoult M, Castro M, Lacaze J 1998 Acta Metallurgica 46 983
[5]
Magnin P, Kurz W 1988 Met. Mat. Trans. A 19 1955
[6]
Favreau J R, Lesoult G, Turpin M 1974 Mem. Scien. Rev. Met. 4
[7]
Stefanescu D M 2007 Met. Mat. Trans. 38 1433
[8]
Mizukami H, Suzuki T, Umeda T 1991 Testu-to-Hagan, 77 134
[9]
Rangel R H, Bian X 1995 Numerical Heat Trans. Part A: Applications 28, No. 5, 589