Astm 536 - Arul

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VOLUME 28

ISSUE 2
of Achievements in Materials June
and Manufacturing Engineering 2008

Analysis of the thixoability of ASTM


A536 ductile iron
M.H. Robert a,*, R. Cristofolini b
a Faculty of Mechanical Engineering, State University of Campinas, Sao Paulo, Brazil
b University of Joinville Region, Joinville, Santa Catarina, Brazil
* Corresponding author: E-mail address: helena@fem.unicamp.br
Received 21.03.2008; published in revised form 01.06.2008

Manufacturing and processing

Abstract
Purpose: Thixoability of the ASTM A536 nodular cast iron is analyzed, it meaning its ability to hold a thixotropic
semi-solid state and to be formed as such. Thixoability can be characterized by the solidification range, fraction
of primary phase and sensitiveness of liquid fraction with temperature (dfl/dT) within the solidification range. It
is also investigated the effect of thixocasting in the microstructure of the considered alloy.
Design/methodology/approach: Differential thermal analysis, differential scanning calorimetry and
thermodynamic calculation package THERMOCALC were used to predict transformations temperatures
involving liquid formation and dfl/dT within the solidification range. Microstructures of thixotropic slurries
produced by partial melting were observed.
Findings: Thixoforming of ASTM A536 nodular iron can be considered in a narrow window of about 28°C,
were some dissolution of graphite nodules can still be afforded; this window meaning the range of temperatures
of co-existence of austenite + graphite + liquid were the eutectic transformation is taking place. At higher
temperatures the dissolution of graphite nodules in liquid can be significant.
Research limitations/implications: Thixoability prediction models rely on sensitive experiments as
thermoanalysis, with results strongly dependent on experimental conditions; and on thermodynamic data,
sometimes not available or reliable for a specific alloy composition.
Practical implications: The prediction of the thixoability of a certain alloy can make it more effective its
thixoprocessing, allows better control of processing parameters and quality of final product; can also subsidize
modifications in the alloy to make it more suitable to semi-solid processing.
Originality/value: The study of the thixoability of a nodular hypereutectic cast iron is an original subject, not
available in the specialized literature, however absolutely necessary if thixoprocessing of this family of alloys
is to be considered.
Keywords: Casting; Thixoability; Thixoforming; Semi-solid alloys

1. Introduction
1. Introduction thixoability, which must gather some criteria such as the
solidification range of the alloy, the liquid fraction at eutectic
temperature, and the sensitivity of liquid fraction with tempera-
With the progress of the semi-solid technology development ture [1, 2]. The first criteria can be limited by the susceptibility of
along the years and the consequent familiarization with the the alloy to hot cracking during cooling if the solidification range
control parameters of the thixotropic slurries fabrication and is too wide; concerning the second criteria, it has been observed
forming processes, researchers and costumers in the field have that more controllable is the processing if eutectic reaction occurs
been finding consensus on some basic requirements for a specific at 30 to 50% liquid and third criteria states that dfl/dT can not be
alloy to be candidate to thixoforming processing. The potential too abrupt, otherwise little changes in temperature lead to big
ability of a certain alloy for thixoforming is characterized by its variation in the liquid fraction and make it difficult to control the

© Copyright by International OCSCO World Press. All rights reserved. 2008 Research paper 115
Journal of Achievements in Materials and Manufacturing Engineering Volume 28 Issue 2 June 2008

process. Results for Al-Si-Cu alloys [3, 4] indicate values of


dfl/dT between 0.007 K-1 to 0.067 K-1 at fl=0.4, depending on the
3. Results
3. Resultsandand
Discussions
discussions
Si-Cu content. It means that an increase of 1K in the alloy
presenting 40% liquid implies in an addition of 0.7 and 6.7 in the 3.1. Thermal
3.1. Analysis
Thermal analysis
fraction of liquid content (%) in the semi-solid; in the first case
(only 0.7 increase in fl/K) thixoability is higher, allowing easier During solidification of a hypereutectic Fe-C system, if Si
manipulation of the alloy in the semi-solid state. content is high, the stable phase graphite is formed as primary
Given the more recent application of the semi-solid phase in the liquid in the solidification range.
technology for ferrous alloys, when compared with the already An important characteristic of Fe-C-Si systems is that eutectic
commercial use of this technology for Al and Mg systems, a little transformation is not isothermal but takes place within a narrow range
has been done so far to establish the thixoability of such family of of temperatures, where austenite, graphite and liquid coexist, as
alloys. Some special classes of steels, such as stainless and tool shown in the general diagram from literature presented in Figure 1.
series have been catching attention and some results can be In the eutectic transformation austenite is formed in the carbon-
available [5, 6]. However, as far as cast iron is concerned, very depleted melt around graphite nodules, encapsulating the primary
little information can be found in the specialized literature, in phase. As transformation proceeds, both graphite nodules and the
spite of the importance of such family of alloys and the potential newly formed austenite grow, maintaining the eutectic transformation
advantages of using semi-solid technology. In one of the available Lo J + G, not in a typical cooperative nucleation-growth, as no new
technical papers [7] it is shown the possibility of producing graphite nodules are formed. In this particular case, the transformation
thinner cast sections of gray iron, via thixocasting process. is not isothermal but occurs in a narrow temperature interval. At
This work investigates the thixoability of the nodular iron ASTM lower temperatures, eutectoid transformation leads to the final
A536, which finds commercial application in the automotive industry structure of the alloy, presenting ferrite and graphite.
as several cast components. The knowledge of the alloy thixoability Thermal analysis shall help to identify solidification range of
can make more effective its thixoprocessing, allowing better control the analyzed alloy, it meaning two distinct regions: one where
of processing parameters and quality of final product. liquid and graphite phases are present, limited by T-liquidus and
the temperature at which eutectic transformation initiates (T5 to T4
in Figure 1); and the eutectic region, where liquid + graphite +
2. Experimental
2. Experimentalprocedures
procedures austenite are present, going from T4 to T3, when the eutectic
transformation finishes.
ASTM A536-60-40-18 (ISO 1693-400-15) nodular iron with Taking the cooling curve from liquid, for example, it should
chemical composition presented in Table 1 was used in this work. show the temperature at which primary solid (graphite) is nucleated,
This alloy is a hypereutectic system, presenting at room tempera- it meaning T-liquidus, the temperatures of eutectic reaction
ture a cast structure containing ferrite and nodular graphite. initiation, with the formation of austenite, and the finishing of
The experiments were divided in two series: study of the
thixoability of the considered alloy and effective production of
samples of thixotropic semi-solid for observations of
microstructure in the thixocast condition.
For thixoability studies, differential thermal analysis (DTA)
and differential scanning calorimetry (DSC) tests were performed.
Curves energy x temperature were taken during heating and
cooling at two different rates: 5 and 10qC/min. From these curves,
temperatures of phase transformations, mainly those involving
liquid formation, and dfl/dT were obtained. To complement
thixoability analysis, it was utilized the software THERMOCALC
to generate the probable phase diagram for the specific
composition used. Informations from the diagram were taken
together with thermal analysis results to discuss the thixoability of
the considered alloy. For THERMOCALC calculations it was
assumed a heating rate of 1qC/min.
Samples of thixotropic semi-solid were produced by partial
melting at different temperatures (from 1140 to 1161qC) and
holding at a constant pre-defined temperature for 30 min followed
by rapid cooling in water. Conventional metallography technique
was used to prepare cross sections for microstructure Fig. 1. General Fe-C-Si diagram (stable) for 2.5wt%Si from literature [8]
observations; Nital 3% was the etching employed.

Table 1.
Chemical composition (wt%) of the ASTM536 cast iron used in the experiments
C Si Mg Mn P S Fe
3.74 2.98 0.05 0.19 0.006 0.01 balance

116 Research paper M.H. Robert, R. Cristofolini


Manufacturing and processing

eutectic reaction or temperature at which no liquid remains, it transformation, or within the T3-T4 interval. In equilibrium
meaning T-solidus. The total solidification range must be conditions it means that 99.7% of liquid is formed by melting of
considered, therefore, the whole interval from fliq = 100% to the eutectic phase. Therefore, as far as thixoforming is concerned,
fliq = 0% or from T5 to T3. the thixoability of the alloy is mostly defined by the sensitiveness
A typical result of thermal analysis of the ASTM A536 of liquid fraction with temperature within this specific range (T3
nodular iron studied is presented in Figure 2. to T4 indicated in the general diagram of Figure 1). At
At low temperatures, it can be observed an inflexion at around temperatures higher than T4, solid fraction is small (light weight
450qC (indicated as A), probably due to stress relief during graphite nodules in dissolution) and it would be difficult to
heating. A more defined peak (B) can be observed around 820qC, control the thixoforming processes. Furthermore, at those high
which can be related to eutectoid transformation (austenite o temperatures the dissolution of graphite can be quick, what must
ferrite + graphite). At higher temperatures, a transformation with be minimized to avoid deterioration of the characteristics of the
significant variation of energy initiates at 1157qC (peak C), nodular iron considered.
followed by small successive peaks until ~1358qC. Repeated tests Therefore, the determination of the eutectic transformation
show similar behavior: a well defined peak starting around 1145- range is fundamental to analyze the thixoability of the considered
1155qC followed by one or two not clearly defined and cast iron. DSC experiments were performed to pursuit this
comparatively lower energy peaks at higher temperatures. objective, as this sort of thermal analysis can be more sensitive to
Data from literature [9] for Fe-C-Si systems indicates T-liquidus energy variations than ATD. Tests were carried out in different
conditions of heating and cooling; several experiments were
higher than 1300qC for alloys with C and Si contents as the ASTM 536.
performed in the same test conditions to make the results more
Therefore, it can be supposed that the initial, high energy
reliable, as DSC is very sensitive to experimental conditions such
inflexion is associated to the eutectic transformation and the
as sample mass, heating/cooling rate, oxidization of the sample,
following small peaks to dissolution of graphite globules and
contact of the material with crucible and so on.
eventual intermetallic phases in the liquid (regardless of their
Typical DSC results are shown in Figure 3, for tests at two
improbable presence for the considered composition).
different heating conditions.
As the composition of the considered iron is close to eutectic,
Fist of all, it can be observed the coincidence of the obtained
during heating most of the liquid is formed in the eutectic
curves, assuring the results reliability. It can be observed the two
main inflexions related to eutectoid (peak B) and eutectic (peak C)
transformations. Table 2 shows transformations temperatures given
by the tangent method applied to the inflexion attributed to eutectic
transformation detected in all curves produced – values presented
correspond to the average for 2 distinct tests in the same condition.
Results obtained in different conditions are quite similar apart
of the influence of cycle type: significant differences were
observed between cooling and heating cycles; this is usually
attributed to different conditions of contact between sample and
crucible walls, either the sample is in solid or liquid state. The
influence of heat transfer on transformations temperatures is less
significant; however the intensity of energy variation in a specific
transformation is higher in tests at the higher rate employed, due
to more difficulty on heat transfer in this condition.
As thixoforming implies in heating of the material from solid
to semi-solid state, it is reasonable to consider results obtained
from heating experiments performed at 10qC/min, a condition less
far from practical. Therefore, eutectic transformation can be
assumed as taking place between 1140 and 1168qC, it meaning a
Fig. 2. DTA signal x T for ASTM A536 nodular iron. Heating narrow window of about maximum 28 degrees for semi-solid
rate: 10qC/min processing, what can make difficult the process control.

Table 2.
Transformations temperatures of ASTM A536 nodular iron, according to DSC analysis, for eutectic range
Cycle type
Temperature Heating Cooling
5qC/min 10qC/min 5qC/min 10qC/min

Ti (ºC) 1140 1140 1141 1140


Tf (ºC) 1161 1168 1122 1116
Ti – temperature where transformation initiates; Tf – temperature where transformation finishes

Analysis of the thixoability of ASTM A536 ductile iron 117


Journal of Achievements in Materials and Manufacturing Engineering Volume 28 Issue 2 June 2008

significantly with temperatures from T4 to T5. It means that on


heating, most of the liquid is formed by eutectic phase melting
within the range of temperatures where eutectic transformation
takes place (T3 to T4).

Fig. 3. DSC signal x T for ASTM A536 nodular iron; different


heating rates: 10qC/min and 5ºC/min

3.2. Phase
3.2. diagram
Phase simulated
diagram by thermodyna-
simulated by
mic calculations
thermodynamic calculations (a)

THERMOCALC commercial software was used to generate


the phase diagram for the specific composition of the cast iron
considered in the work; resulting general diagram and a magnified
detail of the eutectic transformation are shown in Figure 4.
It can be observed that eutectic composition is 3.42wt%C; the
two major phase transformations, eutectoid and eutectic, occur
within a range of temperatures and involve three phases: during
eutectoid transformation austenite + ferrite + graphite co-exist
(therefore a ternary system) and, during eutectic transformation
austenite, graphite and liquid are the phases present in the system.
Detail of eutectic range presented in Figure 4 (b) shows
temperatures of 1152 and 1159qC as beginning and finishing of
melting of eutectic phase in a heating procedure. This range is
narrower than the eutectic transformation range detected in
thermal analysis tests. Moreover, according to the generated phase
diagram, T-liquidus of the considered cast iron is 1260qC; thermal
analysis results did not indicate any transformation at this
temperature. Therefore, values of transformations temperatures
predict by thermodynamic calculation are lower than results
obtained by thermal analysis; this discrepancy can be attributed to
the low heat transfer rate considered in the thermodynamic (b)
calculations, closer to equilibrium conditions (1qC/min).
From obtained data, it was also determined the variation of Fig. 4. Fe-C phase diagram generated by thermodynamic
liquid fraction with temperature, which is shown in Figure 5. As calculations for the composition analysed in this work (ASTM
mentioned previously, as the composition of the studied alloy is A536 nodular iron). (a) general; (b) detail of eutectic
close to eutectic, the liquid content in the system does not change transformation. Heat transfer rate considered: (1qC/min)

118 Research paper M.H. Robert, R. Cristofolini


Manufacturing and processing

minimum liquid fraction where semi-solid can be reliably


processed. In casting operations liquid fractions around 0.6 can be
quite feasible, while for mechanical forming operations
sometimes liquid fractions as low as 0.05 can be the limit, as for
instance in drawing of Al alloys sheets in semi-solid state [10].
The variation of liquid fraction with temperature is not linear:
is lower at the beginning and finishing of the transformation; the
slope of the curve is higher exactly within the processing
windows. So, thixoability material depends on the sensitity of
dfl/dT at processing temperatures: liquid fraction shall not change
drastically with temperatures, otherwise process control can
become critical and even impossible.
Figure 7 presents calculated values dfl/dT for the A536 cast
iron analyzed.

Fig. 5. Variation of solid fraction x T for ASTM A536 nodular


iron, generated by THERMOCALC

Figure 5 shows clearly the massive formation of liquid at


eutectic transformation range (region indicated by the green line),
from the final of eutectic transformation the liquid fraction
variation with temperature increase is negligible (region indicated
by the red line; solid region is indicated by blue line).

3.3. Thixoability
3.3. of ASTM
Thixoability 536 536
of ASTM Fig. 6. Fraction of eutectic phase transformed in liquid x T on
heating of ASTM A536 nodular iron. Suggested thixoforming
Taking in account that on heating ASTM A536 cast iron, most windows (A2 for thixocasting; A1 for thixoforging)
of the liquid is formed within the eutectic transformation interval, it
was determined the variation of liquid fraction x T of the alloy by
calculating the relative areas under the transformation peaks related
to the eutectic transformation obtained in the DSC experiments.
Therefore, it is assumed that the error induced by considering fl =1
at the end of the eutectic transformation (at T4), and not at the actual
T-liquidus (T5 as indicated in Fig. 1), is negligible.
For each specific temperature within the beginning and the
finishing of the transformation, it was calculated the relative area
given by:

Partial area An (Tn – Ti)


fl (n) = (1)
Total area At (Tf – Ti)

where fl (n) = liquid fraction at a generically Tn, is the relation


between the area under the DSC curve limited by Tn and the
temperature where liquid fraction is 0, or the temperature where
transformation initiates (Ti); and the total area under the peak , or
from temperature where transformation initiates and finishes (Tf).
Results are shown in Figure 6. Acceptable processing Fig. 7. Sensitivity of liquid fraction x temperature [dfl / dT] for
windows for thixocasting and thixoforming are suggested in the ASTM A536 nodular iron. Points A and B: values for thixoforming
Figure. Processing window is the range between maximum and at fl = 0.25 [1150ºC] and fl= 0.45 [1154ºC], respectively

Analysis of the thixoability of ASTM A536 ductile iron 119


Journal of Achievements in Materials and Manufacturing Engineering Volume 28 Issue 2 June 2008

It can be observed that dfl/dT is not linear, being higher at their dimension, as thixocast temperature increases. Maximum
intermediate temperatures between beginning and finishing of the reductions around 20% and 40% in number and dimension of
transformation. General results in the presented curve show that in globules, respectively, are observed when heating at the
the whole spectrum of values of temperatures or liquid fractions, maximum thixocast temperature.
dfl/dT varies from around 0.01 to 0.057C-1. In the specific range Taking in account the large holding time of the experiments
suggested for thixoforming two points where picked to exemplify (30 min), the dissolution of the graphite, although an effect to be
the sensitivity of liquid fraction with temperature: points A and B carefully monitored during thixocasting of nodular iron, shall not
in the curve indicate the values for typical thixoforming constitute a limitation for semi-solid processing of such alloys.
temperatures: dfl / dT = 0.044C-1 and 0.056C-1 for fl = 0.25 (at Faster heating and shorter holding time at high temperatures can
1150ºC) and fl = 0.45 (at 1154ºC), respectively. These values avoid excessive graphite dissolution with consequent de-
indicate the need of a close control of thixoforming temperature to characterization of the material properties.
insure the viability of the process.
Studies on Al-Si, Al-Zn-Mg-Cu alloys, considered as
presenting good thixoformability, dfl/dT ranges from as low as
0.007C-1 [3, 11] as mentioned previously. As far as ferrous alloys
are concerned, some literature information reveals values from
0.0097 to 0.02 for Cr-Mn alloy steels [12].
Therefore, thixoforming of ASTM A536 must be looked with
care; however, taking in account the tight control of temperature
on re-heating of billets for thixoforming already achievable using
commercial softwares for induction heating, processing the
studied cast iron in the semi-solid state, although requiring
attention, can be considered.

3.4. Thixocast
3.4. Thixocast microstructures
microstructuresproduced by
partial melting
produced by partial melting

Semi-solid samples of the studied alloy were produced by


partial melting at temperatures within the pre-determined eutectic
range. Typical resulting microstructure is shown in Figure 8 (b);
while (a) shows the original as-cast condition. Thixocast material (a)
presents globular phase, in this case coarse grains of lamellar
martensite, interglobular fine martensite and remaining graphite
spheroids. Globular grains of martensite indicates globular
austenite phase in the semi-solid state, transformed to martensite
by the rapid cooling imposed to the thixotropic slurry.
It can also be observed significant increase in the size of
austenite grains caused by re-heating and holding at high
temperatures. To obtain a semi-solid with thixotropic
characteristics, a proper spheroidization of a solid phase in liquid
environment at thixocast temperatures is required; this
phenomena involves diffusion and, therefore, is time dependent.
On the other hand, diffusion can also promote undesirable growth
of solid phases by coarsening, coalescence, ripening etc., as
observed here and described elsewhere [13]. This effect must be
prevented to avoid excessive growth with consequent
deterioration of rheological properties of the semi-solid. As
austenitic grains are already nearly globular, in this case faster
heating rate and shorter holding times must be preferentially used.
Concerning the graphite phase, it is observed the reduction in
number and dimensions of the globules in the thixocast material,
compared to the as-cast condition, due to their dissolution in the
liquid at the thixocast temperature.
Quantitative analysis of the graphite phase present in ASTM (b)
A536 iron thixocast at different temperatures was performed to
evaluate the extent of graphite dissolution. Results are shown in Fig. 8. Microstructures of ASTM A536 nodular iron; (a) as–cast;
Figure 9 and 10: a reduction of the globules number as well as (b) thixocast by re-heating and holding at 1157qC/30 min

120 Research paper M.H. Robert, R. Cristofolini


Manufacturing and processing

possible the prediction of heating conditions effects on structure


As-cast transformations when producing a thixotropic semi-solid, the
applicability of simulation methods already proved suitable for
conventional heat treatment of steels [15] could be tested for the
partial melting required to produce thixotropic material.
Number of nodules / mm2

4. Conclusions
4. Conclusions

This work shows that, although presenting a wide


solidification range, ASTM A536 nodular iron presents a narrow
window of less than 28qC for semi-solid processing, which
corresponds to the interval where eutectic transformation takes
place and three phases coexist (austenite, graphite and liquid). At
higher temperatures still within solidification range, the solid
phase present (graphite) can dissolve in the liquid, what can lead
to the deterioration of the material properties.
Moreover, in the range suggested for thixoforming, dfl / dT can be
Temperature (qC) substantial, meaning that the liquid fraction in the semi-solid can
change significantly with small changes in temperatures, demanding
attention concerning the control of processing temperatures.
Fig. 9. Variation of number of graphite nodules x thixocast Thermodynamic calculations for temperature transformations
temperature, for ASTM 536 nodular iron. (Holding time at the must be taken with care; it must be remembered that practical
specific temperature: 30 min) conditions are far from equilibrium. Therefore calculated
temperatures and liquid fraction sensitiveness can be significantly
different from those present in practical conditions.
Semi-solid produced by partial melting shows globular solid
phase (austenite) and liquid, a constitution that typically
characterizes a thixotropic semi-solid.
Therefore, considering that a control of temperatures variation
As-cast
Dimension of nonodules (Pm)

within 4 to 5qC is practically viable, thixoforming of ASTM A536


nodular iron, although requiring attention as far as temperature
control is concerned, can be considered as feasible.

References
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