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To cite this article: Abel Tadesse & Hasse Fredriksson (2017): Volume change during the
solidification of grey cast iron: its relation with the microstructural variation, comparison
between experimental and theoretical analysis, International Journal of Cast Metals Research,
DOI: 10.1080/13640461.2016.1277851
Volume change during the solidification of grey cast iron: its relation with the
microstructural variation, comparison between experimental and theoretical
analysis
Abel Tadesse and Hasse Fredriksson
Materials Science and Engineering, Royal Institute of Technology (KTH), Stockholm, Sweden
and they related this expansion with mould material drying furnace for three hours at 200 °C for curing. The
interaction. The use of different types of moulding sand final mould cavity is roughly 50 × 70 × 10 mm width,
also influences the expansion. Green sand mould and height, and thickness respectively.
furan resin mould show differences in expansion dur- Four LVDT sensors mounted in adjustable holes on
ing the eutectic solidification in nodular cast iron, the a rigid frame as shown in Figure 1. Quartz rods were
former method exhibit higher expansion according to used to link the sensor tip with the molten metal in the
Chisamera et al. [12]. mould cavity. The tips of the quartz rods placed inside
Apart from Ref. [1,2,9], the rest adopt uniaxial dis- the mould cavity were shaped like a hook to stick on
placement measurements. In this case, the measurement the surface of the solidifying shell as shown in Figure
cannot be considered as representative of the examined 2(a). The other end of the quartz rods was connected
sample volume. Understanding the volumetric shrinkage to the sensor tip by using connectors. The quartz tube
during the solidification or thermal expansion /contrac- separates the quartz rod from holes in the sand mould
tion will help us to control the alloying elements at the and allows a smooth motion for the rods. The LVDT posi-
same time to provide an additional approach to compen- tioned in all the four faces of the plate at the midpoint
sate or reduce the effect of the micro-shrinkage. There and the thermocouple placed in the geometric centre.
are not many studies presented which analyse the effect These sensors will export the real-time data to a central
of melt treatment on the thermal expansion and con- system during the solidification, except the top and the
traction during the solidification process. In this paper, bottom due to difficulties for pouring and putting the
two types of inoculant were used to study those effect sand mould in a stable position. An insulation material
on the thermal expansion and contraction on a hypoeu- was applied to minimise the heat extraction from the top
tectic grey cast iron (GCI). Then we analysed the linear and bottom parts of the casting. The sensors Channel-1
displacement measurements taken from both the trans- (Ch1) and Ch2 shown in Figure 2(b) measure the surface
versal and longitudinal directions of a thin wall plate, displacement in X–X direction (longitudinal) whereas the
along with temperature-time measurements during the sensors Ch3 and Ch4 measure the centerline displace-
solidification. ment in Y–Y direction (transversal).
In each experiment, around 280 g were melted in a
high-frequency induction furnace (HFIF) inside a quartz
Experimental tube. Argon gas was flashed in and circulates inside the
quartz tube to protect the molten metal from excessive
Thermal expansion/contraction analysis
oxidation. In the case of inoculation experiments, the
All the experiments were carried out in a laboratory scale inoculation was introduced inside the crucible while the
size. One base material (BM) was used in all experiments. melt temperature was kept around 1400 °C. The mag-
A total of eighteen experiments were conducted with netic field created by the induction coil creates a stirring
the help of the Linear Variable Differential Transformer effect on the molten metal and helps the inoculant to
(LVDT) sensors. Except four, the tests were carried out by homogenise throughout the melt.
treating the molten metal with a different weight fraction During the solidification of the alloys in the mould
of inoculant (Table 1). Each condition was repeated at cavity; the LVDT sensors transmit the signal in numeric
least once during the experimental work. A total of seven form and store it on the computer. Simultaneously, the
out of eighteen presented in this paper. The experiments thermocouple sent the temperature signals to the data
not presented are comparable to the results presented logger to record the cooling curve. The setup consists of
here. sand mould, LVDT sensors, thermocouple, rigid frame,
The LVDT experiments were conducted in sand cast- quartz rods and tubes as shown in Figure 1. The accuracy
ing. The sand mould was prepared by mixing 1400g silica of each sensor was ±0.1% of measured data. The temper-
sand and 35 ml water glass (Na2SiO3) as a binder. The ature measurement was done by S-type thermocouple
weight of the binder was determined by considering the with diameter 0.35 mm as shown in Figure 2. The accu-
amount of sand [13,14]. The mould was then kept in a racy of the thermocouple was ±3 °C.
Figure 5. Microstructural evolution upon increasing inoculant percentage from left to right. The first row represent sample with
ASSC inoculant addition, the second row represent sample with MBZCAS inoculant addition. Samples taken from LVDT experiments.
INTERNATIONAL JOURNAL OF CAST METALS RESEARCH 5
Figure 6. Eutectic cells variation. The first row from the second column represent samples with increasing ASSC addition and the
second row from the second column represent samples with increasing MBZCAS addition. Samples taken from LVDT experiments.
LVDT analysis
The volume change during the solidification and cooling
of GCI in a sand mould is shown in Figure 8. The black
line represents the temperature as a function of time.
The dotted and dashed lines show the expansion or con-
traction of the casting and will be discussed later. During
pouring, the temperatures inside the mould increase
and reach the maximum. After reaching the peak, the
temperature starts dropping down to liquidus temper-
ature without involving phase change (I). Precipitation
of austenite begins around 1213.6 °C. The temperature
Figure 7. Calculated austenite fraction (AF) and eutectic cell decreases during the austenite phase transformation (II).
count vs. Carbon equivalent (Ceq). The Ceq increases with Finally, a eutectic solidification starts around 1159 °C.
increasing inoculation amount. After this point the temperature drop and get close
to constant until the end of solidification (III) and then
starts to decrease again after the solidification ends (IV).
For each experiment, the start of austenite precipita-
tion temperature and the start and end of the eutectic
reaction was evaluated, and the results are disclosed in
Table 3.
According to the LVDT results, one gets an expansion
at the beginning depending on the mould expansion
caused by the temperature increase (I). After that, a
contraction during the precipitation of austenite and
expansion during the eutectic reaction occurs (II & III).
Figure 8. Temperature and displacements time curve measured When the solidification completes, contraction will fol-
by thermocouple and LVDT respectively. low during the further cooling (IV). The expansion meas-
urements have been compared with calculation in the
in Figure 14. Samples with 1% MBZCAS inoculant have following way. First, the volumetric changes during the
the smallest fraction of primary austenite compared with eutectic reaction was evaluated from the measurement.
the others. According to the microstructure, the smaller Second, the theoretical calculated was made from the
fraction of primary austenite the larger fraction of the temperature time curve using the relations presented in
eutectic structure is observed. The number of eutectic the Appendix 1. Finally, the thermal contraction during
cells together with calculated austenite fractions is pre- cooling was evaluated and compared with the dilatom-
sented in Figure 7 for comparison. eter measurements.
6 A. TADESSE AND H. FREDRIKSSON
Table 3. Start of primary precipitation, eutectic and end of solidification temperature and time together with average cooling rates
during the austenite and eutectic solidification.
Alloy T𝛾start (◦ C) TEstart (◦ C). TEEnd (◦ C) Δt𝛾 (s) ΔtE (s) ΔT𝛾E ∕Δt𝛾 ΔTEE ∕ΔtE
11a 1217.4 1145.7 1117.6 37.8 84.1 1.897
21b 1216.8 1152.5 1121 39.9 92.6 1.612 0.340
31c 1217 1153.3 1119 39.8 95.0 1.601 0.361
22b 1213.9 1154.7 1122.8 33.1 87.8 1.789 0.363
32c 1213.6 1159 1122.9 34.2 93.9 1.601 0.384
23b 1211.9 1162 1125.2 32.8 93.3 1.521 0.394
33c 1212.3 1163.4 1124.9 30.3 93.9 1.614 0.410
Figure 9. The experimental and calculated volume changes (fraction) during the eutectic solidification. (a) sample without
inoculation, (b–d) samples with 0.14, 0.4 and 1 wt-% ASSC inoculation added, (e–g) samples with 0.14, 0.4 and 1 wt-% MBZCAS
inoculation added respectively.
Figure 10. Linear thermal contraction calculated using data Figure 11. The thermal contraction for different cooling rates
from LVDT measurement between 1080–980 °C. on BM sample in the Dilatometer. The specimen is a round bar
with ϕ3.55 X 19 mm, diameter and length respectively.
The volumetric expansion measured during the
eutectic reaction and the calculated one from the cooling shows that there is a time difference between the ends
curves shown in Figure 9. According to the results, the of the expansion from the measurement and calculated
volume expansion estimated from the cooling curve are value and the former have the higher total volumetric
smaller and ends earlier than the measurement. Figure 9 changes. For samples with MBZCAS, the theoretical and
INTERNATIONAL JOURNAL OF CAST METALS RESEARCH 7
Table 4. Latent heat of fusion during the solidification; latent heat evaluated from the cooling curve by considering the area under
the first derivative and the zero curve during the solidification interval, latent heat generated in Thermo-Calc by considering carbon,
silicon and manganese contents.
Latent heat in* Latent heat in†
Eutectic
Alloy Heat of Fusion* Heat of Fusion† Austenite precipitation Eutectic growth Austenite precipitation growth
11a –269.34 –266.01 –85.17 –184.17 –110.78 –155.23
21b –246.19 –262.96 –74.18 –172.02 –109.76 –153.2
31c –251.25 –262.8 –75.76 –175.49 –108.24 –154.56
22b –231.55 –258.4 –62.22 –169.33 –102.66 –155.74
32c –241.37 –253.33 –65.89 –175.48 –99.62 –153.71
23b –216.23 –247.24 –55.67 –160.56 –89.47 –157.77
33c –227.18 –241.66 –55.31 –171.87 –79.32 –162.34
*from cooling curve [J/g]; †from Thermo-Calc [J/g].
Table 5. The comparison between the calculated, measured densities and volume changes with the corresponding percentage
errors.
Density [g/cm³] Volume changes [%]
Alloy measured calculated Error [%] measured calculated Error [%]
11a 7.294 7.246 0.658 2.4 3.103 0.703
21b 7.229 7.242 0.180 2.4 3.071 0.671
31c 7.252 7.243 0.124 2.15 3.090 0.94
22b 7.135 7.237 1.430 1.5 3.018 1.518
32c 7.252 7.237 0.207 2.5 3.036 0.536
23b 7.059 7.232 2.451 2.1 3.022 0.922
33c 7.017 7.229 3.021 3.2 3.048 0.152
experimental values are close to each other and have The comparison was made between latent heat from
higher experimental volumetric expansions compared cooling curve and Thermo-Calc by considering carbon,
with ASSC. The eutectic cell count also shows that there silicon, and manganese as the main constituents. The
are more cells in samples with MBZCAS than in samples latent heat does not change that much as the inocula-
with ASSC (Figure 7). tion weight percent increases according to the Thermo-
Figure 10 shows the linear thermal contraction calcu- Calc result. However, the cooling curve measurement
lated from the LVDT displacement measurements after from the experiment shows a difference between each
the solidification for temperature ranges between 1080 other. The differences emphasize that the latent heat
and 980 °C (Appendix 4). The sample without inocula- involved during the solidification was different. From
tion has the lowest linear contraction in longitudinal and both methods, one can see that when the carbon equiv-
highest in the transversal directions of all sand casting. alent increases the latent heat decreases. The decrease
Though, the rest of the sand casting shown in Figure 10 is mainly related to the decrease in latent heat involved
displays a decrease in contraction with an increase in during the austenite precipitation at the early stage
inoculation until it reaches 0.4 wt-% and then increases (Table 4).
at further addition. Samples with higher inoculation These results indicate that the number of lattice
display more or less large linear contraction in both Ch defects increases as a result of increasing the inoculant
[1–2] and [3–4]. The comparison of thermal contraction fraction. An increase in lattice defects increase the num-
after solidification for sand casting with the dilatometer ber of holes in the lattice for carbon atoms. Thus, more
measurements shows that latter method has a lower carbon might be presented in the austenite; these phe-
contraction than the former (Figures 10 and 11). nomena will allow the extra carbon in the austenite to
precipitate as graphite in the later stage of solidification
and during cooling after solidification. As a result, more
Latent heat estimation
expansion occurs after the solidification completed, as
The Newtonian law of heating and cooling method was shown in Figure 8.
applied in the area between the first derivative of the
cooling curve and the zero curve to estimate the latent
Dilatometer measurement
heat during the solidification [17,18]. The latent heat
decreases as the inoculant amount increases as per the The contraction measurement during cooling from the
results. Alloy 11a has the highest latent heat (269 J/g). dilatometer for various cooling rates are presented in
Alloy 23b has the lowest latent heat (216 J/g). Increasing Figure 11. The contraction coefficient decreases from
the weight percentage of ASSC and MBZCAS decreases 5E-5 to 1.5E-5 with decreasing in temperature. Upon
the latent heat. The decrease in latent heat is larger for decreasing the cooling rate, the linear thermal contrac-
samples with ASSC addition. tion coefficient changes. The expansion or contraction
8 A. TADESSE AND H. FREDRIKSSON
along the diameter in the dilatometer experiment is neg- decreases. The random errors of each measurement were
ligible since the length is much longer than the diameter. calculated by considering the accuracy of the measur-
By taking this into account, the volumetric contraction ing equipment’s and included in Figure 12 to bound the
in percentage can be calculated for comparison with the maximum and minimum error limits.
dilatometer measurement for each cooling rates when
the temperature drops from 1080 to 980 °C. The max-
imum and minimum volumetric contraction between Discussion
this temperature interval evaluated from the dilatometer The microstructure evolves by modifying the solidifica-
measurement was 0.34% with a cooling rate of 1 K/Min tion pattern with melt treatment. The inoculants create
and 0.236% at a 30 K/min. According to the result, as a large number of stable oxides or sulphides nuclei prior,
the cooling rate decreases the volumetric contraction or during the solidification process [1,2,19]. These nuclei’s
increases. This result clearly indicates an increase in favour the inoculation of eutectic cells and increase the
cooling and heating rate will influence the total volume number of growing cells. The larger the number of cells
change. are the slower will the growth rate for each cell be. The
However, a comparison between the volume changes lower the growth rate is, the coarser the structure will
according to Appendix 3 calculated from densities and be. Thus, one could expect that the structure of each
changes of the volume fraction of graphite with temper- cell will be coarser the larger the cell number is. This is
ature shows a reasonably good correspondence with the what has been observed in the microstructures of LVDT
measurements represented in Table 5. experiments and explains the transition from under-
cooled to flake graphite by increasing melt treatment.
Density variation The lower growth rate will also decrease the undercool-
ing temperature during the solidification process in the
The measured densities of the LVDT samples show vari- eutectic region.
ation with the melt treatment as described in Figure 12. The displacement measurement shows that the
The result indicates that by increasing the melt treatment expansion during the solidification process continues
with both ASSC and MBZCAS the density of the final cast to a certain level after the solidus point. A deviation
Figure 13. Maximum displacement measured by LVDT after solidification ends. (a) and (b); the displacement measurement vs.
change in carbon equivalent by adding ASSC and MBZCAS inoculants respectively. TDS1,2 and LDS1,2; transversal (Ch3,4) and
longitudinal (Ch1,2) displacements along the opposite sides respectively.
INTERNATIONAL JOURNAL OF CAST METALS RESEARCH 9
[18] Stefanescu DM. Thermal analysis – theory and applications and the mass balance should be considered. The heat
in metalcasting. IJMC. 2015;9(1):7–22. balance becomes;
[19] Muhmond HM, Fredriksson H. Relationship between
inoculants and the morphologies of MnS and graphite dQ∕dt = (V × 𝜌eut × ΔH eut × dfeut ∕dt) (4)
in gray cast iron. Metall Mater Trans B. 2012;44B:283–298.
[20] Elmquist L, Diószegi A. Relation between SDAS and where ΔH eut is the heat of solidification of eutectic, dfeut/
eutectic cell size in grey iron. Int J Cast Met Res. dt is the volume fraction change of eutectic per change in
2010;23(4):240–245. time, 𝜌eut is the density of eutectic.
[21] Jabbari MM, Davami P, Varahram N. Effect of cooling rate
on microstructure and mechanical properties of gray cast The first part of Equation (3) is neglected in (Equation 4),
iron. Mater Sci Eng A. 2010;528(2):583–588. since the heat of solidification is around 400 times Cp and
[22] Stefanescu DM. Science and engineering of casting the temperature variation is very small during the eutec-
solidification. New York (NY): Springer; 2015. p. 485–492. tic growth. Hence the heat transfer expressed with heat of
[23] ASM ready reference. Thermal properties of metals. fusion.
p. 9–13; 2002. Materials Park, Ohio (US): ASM International.
From mass balance;
[24] Angus HT. Cast iron: physical and engineering properties.
London: Butterworth & Co.; 1978. p. 112–123.
fgreut = 1 − f𝛾eut (5)
Appendix 1. Theoretical background where fgreut and f𝛾eut are the fraction of graphite and austen-
The theoretical parts mainly focused on the solidification. It ite in the eutectic solid respectively, this can be taken from
considers the three main parts; parts with no phase changes phase diagram.
occur at the beginning, a region where austenite precipitation
occurs and the eutectic solidification region. Thermo-physical 𝜌eut = fgreut × 𝜌gr + f𝛾eut × 𝜌𝛾 (6)
properties are shown in Table 7.
By combing Equations (2) and (4)–(6) in the eutectic for-
• The slope of a temperature-time curve in the first stage
mation region, the fraction of eutectic can be calculated.
can be referred as the cooling rate. In this part, the
molten metal cool down without a phase change; the
𝜌 = 𝜌l × 1 − fs + fs × (fgr(𝛾+eut) × 𝜌gr + f𝛾(𝛾+eut) × 𝜌𝛾 )
( )
liquid is considered to be in the superheat region. No (7)
solidification occurs.
where 𝜌 the density of system contains solid and liquid,
Hence the heat balance becomes; fs = f𝛾 + feut, fgr(𝛾+eut) is the fraction of graphite in primary
austenite plus eutectic, f𝛾(𝛾+eut) is the fraction of austenite in
dQ∕dt = V × 𝜌l × Cp × dT ∕dt (1) primary austenite plus eutectic.