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2012 IOP Conf. Ser.: Mater. Sci. Eng. 27 012064
(http://iopscience.iop.org/1757-899X/27/1/012064)
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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
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.
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)
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
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
(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