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Nanoausferritic matrix of ductile iron

D. Myszka, K. Wasiluk, E. Skoek & W. Świątnicki

To cite this article: D. Myszka, K. Wasiluk, E. Skoek & W. Świątnicki (2015) Nanoausferritic
matrix of ductile iron, Materials Science and Technology, 31:7, 829-834, DOI:
10.1179/1743284714Y.0000000733

To link to this article: https://doi.org/10.1179/1743284714Y.0000000733

Published online: 08 Dec 2014.

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Nanoausferritic matrix of ductile iron
D. Myszka1, K. Wasiluk*2, E. Skołek2 and W. Świa˛tnicki2
Austempered ductile iron is known for its excellent mechanical properties resulting from special
phase composition and austempering heat treatment. Typical microstructure consists of ferrite
plates of micrometre size submerged in untransformed austenite matrix. It has been recently
shown that by use of appropriate chemical composition of cast iron and well targeted heat
treatment parameters, it is possible to reduce ferrite plate’s width to submicron or even
nanometric size. This creates the potential to achieve even higher mechanical properties of
austempered ductile iron. The paper describes the influence of applied heat treatment
parameters on microstructure of selected austempered ductile iron grades. Conditions necessary
to reduce size of phases to a nanometric scale by heat treatment in austempered ductile iron are
discussed.
Keywords: Ductile iron, Austempering, Nanostructure, Ausferrite

This paper is part of a special issue on Modern Steels 2014

Introduction ductile iron matrix assuming a completely ausferritic

Austempered ductile iron (ADI) is a structural material
that constantly arouses the curiosity of researchers and
interest of practitioners: designers, users and foundry-
men. This is probably the reason why new ideas and
studies emerge all the time aiming mainly at an
improvement of its properties.1,2 This is particularly
important in terms of the ADI implementation and use.
It is enough to mention that since 2000 its production in
the world has been increasing by an average of about
20 000 t per year.3,4 This demonstrates the great interest
of the users of castings made in ADI, which is a popular
material for machine parts and equipment operating in
the sectors of industry, such as automotive, railway,
agriculture, defence, etc.
In this ductile iron, the ausferritic matrix is obtained by
the austenitising and austempering treatment carried out
under the specific conditions of time and temperature. The
microstructural analysis of ausferrite morphology leads to
the conclusion that there are several distinct features
directly dependent on the time of isothermal transforma-
tion within the range of temperatures between Ar1 and Ms.
When the transformation time is very short, the ductile
iron has an almost completely martensitic matrix with
only traces of the lamellar ferrite precipitates (Fig. 1a).
This is due to complete transformation of the thermally
unstable austenite into martensite during final cooling to
ambient temperature. The longer times of transformation
increase the ferrite fraction in the form of packages of
plates separated by austenite (Fig. 1b). Further transfor-
mation leads to austenite stabilisation. The result is the
1
Warsaw University of Technology, Faculty of Production Engineering,
Warsaw, Poland
2
Warsaw University of Technology, Faculty of Materials Science and
Engineering, Warsaw, Poland
*Corresponding author, email kamil.wasiluk@nanostal.eu
structure and containing austenite in two forms: austenite
layers separating the plates of ferrite and blocks of
austenite located between the ferritic–austenitic packages
(Fig. 1c). The austenite stability is also affected by
graphite nodularity as higher fraction of graphite nod-
ules leads to greater stability of retained austenite.5 A very
long time of isothermal transformation, taking place
within the most commonly used temperature range of
250–400uC, usually leads to the formation of typical
bainitic microstructure.
The analysis shows that with the progressing time of
isothermal transformation, austenite undergoes thermal
stabilisation and the Ms temperature drops down.6–8
Therefore, a diagram shown in Fig. 2 can be sketched,
allowing for all of the above mentioned microstructural
conditions. The diagram neglects the values of the time
and temperature of isothermal transformation, but as
the results of experiments show, the general trend in Ms
temperature changes is similar for all ADI types in the
range of 250–400uC.
The time of isothermal transformation is one of the
most important parameters controlling the ductile iron
matrix during heat treatment. Calculating the best time
of isothermal transformation, from the point of view of
the desired cast iron properties, is a very difficult task.
Typically, it is determined by carrying out a large
number of the heat treatment operations and testing the
mechanical properties in correlation with the time–
temperature–transformation (TTT) diagrams.9
The increase in strength parameters of ADI may be
obtained by formation of a proper content of phases and
refinement of ausferritic matrix.14 Moreover, to ensure
the resistance to cracking, the ausferritic matrix should
be free from the hard and brittle carbides or martensite.
It means that the isothermal transformation should be
carried out until austenite gets saturated with carbon to
a degree such that it will reduce the Ms temperature to a

ß 2015 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 1 September 2014; accepted 25 November 2014
DOI 10.1179/1743284714Y.0000000733 Materials Science and Technology 2015 VOL 31 NO 7 829
Myszka et al. Nanoausferritic matrix of ductile iron

1 Microstructure of ausferritic ductile iron matrix after time of isothermal transformation amounting to a 5 min, b 30 min
and c 120 min: a9, martenite, ab, bainitic ferrite, cf, austenite films, cb, blocky austenite; conditions indicated in Fig. 2
as A, B and C

alone. For this, it was necessary to determine the proper

time of isothermal transformation, in addition to proper
undercooling in the first phase of the process, which are the
critical factors for ultimate refinement of the ausferritic
structure.

2 Schematic representation of temperature changes dur-
ing heat treatment shaping ductile iron matrix (changes
in Ms temperature during isothermal transformation)
point below room temperature. When this happens, the
material will still contain a small amount of the
mechanically unstable austenite, supporting the process
of hardening during the experimental and technological
operations.10–14
It has been reported that in steels containing increased
amount of carbon and silicon, it is possible to obtain a
high strength and toughness by heat treatment inducing
the isothermal transformation of austenite into a mixture
of carbide free bainitic ferrite and carbon enriched
austenite,15–17 both phases of nanometric dimensions.
The aim of this work is to obtain a nanocrystalline
ausferritic structure in two types of ductile iron containing
the additions of copper with molybdenum or molybdenum
Table 1 Chemical composition of examined ductile iron (wt-%)
Methodology
Studies were carried out on ausferritic ductile iron with the
chemical composition shown in Table 1. The test samples of
a cylindrical shape with a diameter of 3 mm and a length of
10 mm were cut out from the examined material by
electrical discharge machining. Using a quenching dilat-
ometer, the characteristic temperatures A1?3 and Ms were
determined, and phase transformations occurring at differ-
ent temperatures during the process of austempering were
examined for both tested cast irons. Using the obtained
dilatometric data, the TTT diagrams were plotted for the
range of bainitic transformation. Sections were prepared,
from the samples treated at temperatures comprised in the
range of the formation of upper and lower bainite, for
metallographic examination by light microscopy and SEM.
Additionally, from samples treated in the lower range of
bainitic transformation, thin foils were cut out for TEM
examinations in the bright and dark field conditions.
On the basis of the TEM images, the thickness of the
ferrite plates and of the austenite layers was determined
in accordance with the following stereological formula18
2
d~ L (1)
P

Material C Si Mn S P Mg Cu Mo

ADI_CuMo 3.40 2.80 0.28 0.015 0.035 0.055 0.72 0.27

ADI_Mo 3.50 2.54 0.16 0.013 0.041 0.047 0.01 0.24

830 Materials Science and Technology 2015 VOL 31 NO 7


3 TTT diagram for ADI_Mo
where ‘d’ stands for the real size of the element of the
microstructure (in the analysed case the real thickness of
a plate) and ‘L’ means the size of the microstructure
element measured in the TEM image (in this case, the
plate width measured on the image). The plate widths
(L9) were measured perpendicularly to the interphase
boundaries.
Results and discussion
The TTT diagrams obtained through dilatometric study
(Figs. 3 and 4) show various phase transformations
taking place in the examined cast iron, enabled tracing
4 TTT diagram for ADI_CuMo
Myszka et al. Nanoausferritic matrix of ductile iron
changes in the cast iron microstructure during heat
treatment. From Figs. 3 and 4, it is clearly visible that
for both examined ADI irons, two overlapping C curves
are present within the temperature range between Ar1
and Ms in TTT diagrams. The upper and lower C curves
correspond to formation of upper and lower ausferrite
respectively.
The most interesting results were obtained in the
analysis of microstructure images of cast iron matrix in
both upper and lower ausferrite range (Figs. 5 and 6).
The detailed observations by the use of TEM revealed
that the upper range of transformation is characterised
by an increasing amount of the ferrite plates of an
Materials Science and Technology 2015 VOL 31 NO 7 831
Myszka et al. Nanoausferritic matrix of ductile iron
a proper microstructure of ADI_CuMo matrix: austenite and ferrite; b bainite in ADI_Mo iron matrix after long time of iso-
thermal transformation
5 ADI microstructure after short and long time of transformation in upper ausferrite range
6 ADI_Mo matrix microstructure after very long time of
transformation in lower ausferrite range (72 h)
irregular structure (Fig. 7), which after certain time
undergo transformation into a typically bainitic struc-
ture (Fig. 5b). In the lower range, the plates of ferrite are
similar in their morphology to needles. The transforma-
tion at low temperature with a sufficiently long time
promote the formation of structure with a nanometric
thickness of the ferrite plates (Figs. 8 and 9).
The thickness of ferrite plates in ADI_CuMo iron
austempered in 250uC for 10 h (Fig. 8) varies from 15 to
434 nm, with the mean value of 117¡8 nm. The plates
were separated by retained austenite films with thickness
varied from 8 to 258 nm; (mean thickness value was
52¡4 nm). Small blocks of austenite were also observed
in microstructure. Overall volume fraction of austenite
determined by stereological analysis is 37?1¡4?6%.
Ausferrite structure of ADI_Mo austempered at 320uC
a bright field; b dark field (austenite reflexes)
7 Feather-like shaped plates in ADI_Mo matrix
832 Materials Science and Technology 2015 VOL 31 NO
for 36 h (Fig. 9) is distinctly finer. Mean ferrite plates
thickness is 63¡6 nm within range from 26 to 173 nm.
The austenite appeared in form of layers; between ferrite
plates, no blocks were observed. The thickness of
austenite varied from 8 to 166 nm, with a mean value
of 50¡5 nm. Volume fraction of austenite is 32?6¡5?0%.
Results of the stereological measurements of the size of
phases present in both kinds of cast iron subjected to
austempering at various temperatures are summarised in
Table 2. Microscopic observations confirm that in low
range of austempering, temperatures with increasing time
of the treatment (to certain critical time) has beneficial
effect to the fine, typical ausferrite structure formation.
In both types of cast iron, it is easy to notice differences
in the duration of bainitic transformation. In the lower
range of ausferrite, in the cast iron containing copper and
molybdenum and in the cast iron containing molybde-
num alone, the times of transformation are 16?6 and 7 h
respectively. Moreover, in the lower range, the time to
end the bainitic transformation is shortest at about 260uC
for ADI_CuMo and 300uC for ADI_CuM. On the other
hand, in the upper range of ausferrite, the minimum time
to stop the transformation is similar for both ADI_CuMo
and ADI_Mo, and amounts to 17 min. This minimum
time is acquired for 480uC in both alloys studied. In this
range, the decrease of temperature prolongs the time
necessary to end the transformation.
An important fact to which attention should be paid is
the different Ms temperatures for the two types of cast
iron. For the copper and molybdenum containing cast
iron, the Ms point is 225uC, while for the cast iron with
0?27% molybdenum alone, it is 180uC. This indicates
that, in the case of cast iron with the addition of
7
 Myszka et al. Nanoausferritic matrix of ductile iron

a bright field; b dark field (austenite reflexes)

8 ADI_CuMo matrix structure obtained by isothermal transformation proceeding for 10 h at 250uC

a bright field; b dark field (austenite reflexes)

9 ADI_Mo matrix structure obtained by isothermal transformation proceeding for 36 h at 320uC

Table 2 Size of phases present in both types of cast iron subjected to austempering at various temperatures

Width of bainitic Width of retained Austenite blocks Austenite volume

ferrite plates/nm austenite layers/nm area/mm2 fraction/%

Range Average Range Average Range Average

ADI_Mo 320uC–36 h 26–173 63¡6 8–166 50¡5 Lack 32.6¡5

ADI_CuMo 250uC–10 h 15–434 117¡8 8–268 52¡4 0.35–3.66 37.1¡4.6

molybdenum alone, substantial undercooling in the first Acknowledgements

step of austempering, even down to 180uC, is not able to
initiate the martensitic transformation. Conducting the
process of austempering at a temperature so low for a
time sufficiently long to complete the transformation
with stabilisation of remaining austenite, could promote
the formation of an extremely fine mixture of ferrite and
austenite.
Conclusions
The results presented in this paper have been supported by
the project ‘Production of nanocrystalline steels using
phase transformations’ – NANOSTAL (contract no.
POIG 01?01?02-14-100/09 with the Polish Ministry of
Science and Higher Education). The project is cofinanced
by the European Union from the European Regional
Development Fund within Operational Programme
Innovative Economy 2007–2013.

The results presented hereby show that it is possible to

obtain in cast iron an ausferritic structure with nano-
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