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Dirisiotr of Malerials Engiv7rcring. School IJ/ Applied .%icncr. Nuyatg Tecl7iiolctgic~al Ut7icersil~~, Sit7guporc 09798, Sittguporr
-._
Abstract
The effects of the Ti:B ratio, the meit holding temperature and the melt mechanical agitation on the performance of aluminum
grain refinement master alloys were investigated using small ingot castings. The results confirm that the presence of dissolved Ti
in the melt is the key factor for effective grain refinement. omogenizing the distribution of heterogeneous nuclei in the melt by
mechanical agitation can further enhance the performance of Ti-B based master alloy. When the amount of disso!ved Ti in the
melt is less than the peritectic point, the columnar uiaxed transition in master alloy treated melt is more sensitive to heat
transfer variation rather than to the number of Ti particles retained in the melt. Slow cooling is recommended to avoid
columnar growth. As the holding temperature increases, inoculation fade occurs. 0 1937 EIsevier Scieace §.A.
Table 1
Chemical compositions of commercially pure Al and the Ti-AI and B-Al master alloys (wt.‘%)
Element
-
Fe Si Mg Ga V Ti I3 Misc. Al
-.
Pure Al 0.110 0.058 0.001 0.014 0.01 I 0.025 Bal.
Ti-Al 0.2 IOk 1.0 0.03 0.03 Bal.
B-Al 0.30 0.20 0.05 5 + 0.5 0.03 Bai.
In the pre;ent work, the effects of the holding tem- min for 1 h to ensure dissolution of the master alloy,
perature, mechanical agitation and the cooling rate and then allowed to solidify in still air for subsequent
on the performance of the master alloys is investi- metallographic examination.
gated in addition to those of the Ti and B contents, Five 100 g ingots with a fixed amount of master
through small ingot casting. alloys additions (0.125 wt.% Ti and 0.005 wt.% B;
Ti/B atornic ratio 6:l) were also cast at different
holding temperatures of 725, 800, 850, 900 and 95O’C
2. Experimental respectively. The alloy addition, holding time and
casting procedures were the same as described above.
All experiments were conducted on 100 or 200 g Two 200 g ingots with the same 0.125 wt.% Ti and
commercially pure aluminum ingots cast in graphite 0.005% B addition (Ti/B atomic ratio 6: 1) were cast
crucibles. A master alloy of nominal composition 10 with and without additional mechanical stirring just
wt.% Ti which contained flaky TiAl, particles was before the solidification of the ingot. All other
used to add Ti whilst a 5 wt.% B master alloy was parameters were as described earlier, except for the
chosen for the B addition. The composition of the stirring operation. One melt was taken from the fur-
commercially pure Al and the B-Al and Ti-Al mas- nace at 725°C and allowed to solidify in air without
ter alloys is given in Table 1. Note that this proce- any agitation, whilst the other melt was taken out
dure is different to reported procedures in the from the furnace at the same temperature and imme-
literature where Tibor master alloys are added which diately stirred before solidification. The cooling curve
contain both Ti and B in one master alloy, pre- of the melts were determined using a K type thermo-
added, in pre-determined amounts. couple and a chart recorder. The stirring was carried
Experiments were carried out to examine the effects out using an alumna rod and lasted for 15 s. Stirring
of four processing parameters, namely the Ti/B ratio, stopped when the melt reached 700°C, the melt then
superheating, the cooling rate and stirring, on the so- being allowed to cool down to the melting point and
lidification structure of the ingots. solidify in air.
Four 100 g ingots were cast with different Ti/B The ingots were sectioned through their centre
ratios, an aluminum ingot without inoculation treat- lines, which later were then polished and etched to
ment also being produced as a reference. The propor- reveal their grain structures. Metallographic specimens
tion of master alloys used in the investigation is given were taken from the centre of each ingot at the cross-
in Table 2. Aluminum melts were superheated to section for microscopic studies. Poultant’s regent con-
725°C in the crucible by a resistance furnace, and taining 30 ml HCl, 15 ml of HN03, 2.5 ml of 40%
then pre-weighed master alloys were added. The melts HF and 2.5 ml of distilled water was used for
were stirred with an alumina rod at intervals of 15 macrostructure etching. Photomacrographs and pho-
tomicrographs were taken at the cross sections of in-
gots using a 35 mm camera with a macro-zoom lens,
Table 2
and a stereo microscope.
Proportion of Ti and B used in the 100 g i -got castings Grain size measurements were carried out on the
etched specimens. The linear-intercept method was
Sample Wt.% of Ti Wt.‘% of B Atomic ratio Ti/B used in which a test line of length L was drawn
randomly on the sample in different directions. The
1 0.150 0
length of the line varied, depending on the grain size
2 0.125 0.005 6/l (whole number)
3 0.050 0.020 l/2 (whole number) of each ingot. The number of grains intercepted was
4 0 0.030 - counted. For each sample, 6 test lines at different
directions were drawn for grain size measurement.
‘55
z UL
65 90 115 140 165 190 215 240 265 290
Superheatin? Temperature I Degree C
4.1. The grain refinement mechanism leaving less particles suspended in the melt. The down-
ward rate of these particles is a function of the particle
The essence of grain refinement inoculation is to diameter and the viscosity of the melt, described by
promote the columnar-to-equiaxed transition during Stokes’s Law. Upon solidification, a large amount of
solidification of a casting. Several models have been TiB2 particles accumulated at the edge and the bottom
proposed for this transition, of which Hunt’s steady of the melt produced a lot of heterogeneous nucleation
state model [15] gives the best insight to the transition sites, resulting in finest grains. Since less TiBz particles
in a simple formulation. Three parameters are recog- were present at the centre of the melt during solidilica-
nised by Hunt’s model as influencing this transition: tion, the average grain size is larger there. Mechanical
alloy composition, nucleation undercooling and nucle- agitation redistributes the TiB2 particles and provides a
ation site density. In the present studies, the alloy large number of particles throughout the whole melt, as
composition has remained unchanged except for the a result an overall better grain refinement being
different levels of Ti and B and hence this variable does achieved. The results in Fig. 3 show clearly that hetero-
not exist. The solidification rates also were essentially geneous nucleation played a major role in grain refine-
constant, particularly through the solidification temper- ment. A greater melt holding temperature decreases the
ature range, and hence the nucleation undercooling viscosity of the melt and reduces the number of hetero-
during solidification could only be influenced by the geneous nucleation sites suspended in the melt, result-
inoculation. ing in the inoculation fade shown in Fig. 3.
Results in Fig. 1 reveal that when the atomic Ti/B The appearance of columnar grains at the top of
ratio is kept at 1:2 or less in the ingot, the effectiveness each in.got can be attributed to enhanced heat transfer
of grain refinement is poor. As a matter of fact when dur!ng ingot solidification. When ingots start to cool
the atomic ratio Ti/B is equal to or less than 1:2, all of down and solidify, the heat removal rate will be great-
the Ti will be consumed in forming stable TiB, which est at the open top of the melt where the liquid metal is
has a large enthalpy of formation of 326.41 kJ mol - l. exposed directly to room-temperature air. The relatively
In this case no dissolved Ti is left in the melt, resulting high heat removal rate at the top surface of the melt
in very limited grain refinement. The addition of 0.15 will in turn increase the temperature gradient in the
wt.% Ti alone can significantly reduce the average grain melt, promoting columnar grain growth. Mechanical
size of the ingot. The presence of a small amount of B agitation that redistributes TiBz particles, however, will
can achieve even better grain refinement. In other not affect Ti dissolved in the melt. An enlarged view of
words, retaining a small amount of dissolved Ti in the the ingots is shown in Fig. 4. It is evident that mechan-
aluminum melt is the key requirement for effective ical agitation only slightly reduced the grain size in the
grain refinement. ingot top columnar zone, and did little in promoting
Both ingots shown in Fig. 3 contain combined 0.13 columnar-equiaxed transition. This result indicates
wt.% Ti and B. The atomic Ti/B ratio is 6:1, indicating strongly that the change in the number of TiBz particles
that both TiB2 intermetallic particles and dissolved Ti in front of the advancing columnar-melt interface does
are present in the melt during ingot solidification. TiB,, not have any signifirant influence on columnar-
as a intermetallic phase in the aluminum melt, has a equiaxed transition as long as the amount of dissolved
density of 4.48 g cm- 3, which is significantly greater Ti remains the same: this is because the total amount of
than that of aluminum at 2.70 g cmd3. During the Ti addition to the melt was 0.125 wt.%, which is less
holding time, TiB2 particles will tend to move down- than the peritectic point shown in Fig. 5. After the
wards and settle at the edge and bottom of the ingot, formation of TiB,, the dissolved amount of Ti was
direct contact with hot emcible waI1, resulting in a
erature gradient in the melt during solidifica-
Cc)). Equiaxed grain nucleation will start