Inclusion measurements in Al–6Si alloys

using liquid metal cleanliness analyser

technique
S. A. Al Kahtani*
The present study was undertaken to investigate the capability of the liquid metal cleanliness
analyser (LiMCA) technique for measuring different types of inclusions in commercial pure
aluminium and Al–6Si casting alloys. The main purpose of the study was to evaluate the technique
in the case of casting alloys, where the inclusion levels are considerably higher than those found
in wrought aluminium alloys for which the LiMCA has generally been used to date. The inclusion
types studied included Al2O3, Al4C3, MgO, CaO, TiB2 and TiAl3, representing inclusions typically
found in aluminium casting alloys. The inclusion additions were made using powder, master alloy,
pure metal and metal matrix composite sources. In the case of powder inclusions, the inclusions
were injected into the alloy melt using a powder injection technique to prepare inclusion
containing ingots, which were subsequently used for inclusion addition to fresh alloy melts to
conduct the LiMCA tests. Microstructural examination of solidified samples obtained from the
LiMCA probe tube used for the measurements and from samplings of the melt was also carried
out using optical microscopy and electron probe microanalysis.
Keywords: Inclusions and oxides, LIMCA, MgO, CaO, Al4C3, Al2O3, Al4C3, TiB2, TiAl3

Introduction non-uniform distribution of the inclusion particle sizes,

additional complexities are introduced.3,4
The common types of inclusions in aluminium alloys are Several qualitative and semiqualitative techniques are
oxides, nitrides, carbides, fluorides and borides. Oxide being used to estimate and control the inclusion
films are also commonly observed and are generated concentrations in aluminium castings. Included among
during the melting process when the melt surface these techniques are some very sophisticated (and
becomes oxidised due to its contact with the surround- expensive) electronic devices that characterise the
ing atmosphere. Such oxide films are located on the melt volume, size and distribution of inclusions suspended
surface and can become entrapped within the melt in a melt, and on the other end of the scale, the simple
during stirring, alloying or other melt treatment proces- shop floor reduced pressure test, which is the foundry
sing. Table 1 lists the different types of inclusions standard often used for measuring the hydrogen level
observed in molten aluminium, their size and morphol- and, indirectly, the inclusion level in aluminium melts.5
ogy.1,2 The control of metal cleanliness in molten The liquid metal cleanliness analyser (LiMCA) system
aluminium alloys requires monitoring and minimising is designed to measure the concentration and size
the presence of impurities such as non-metallic inclu- distribution of non-conductive particles suspended in
sions and hydrogen to the lowest concentration levels. A molten aluminium. The LiMCA unit consists of a probe,
number of techniques have been developed for the a current source and a signal processing system. The
determination of melt cleanliness. These range from probe consists of two electrodes and a sampling tube
qualitative to quantitative techniques, as well as made of non-conducting material (alumina silicate),
analytical laboratory procedures. Owing to the relatively having a small orifice (,300 mm) near its bottom. The
low concentrations of inclusions normally present in tube is immersed in liquid metal, and by applying
the melt, a precise estimate of the inclusion levels is a vacuum or pressure, the liquid metal can be made to
rather complicated task. Furthermore, because of the flow into or out of the tube through the orifice. A
constant electric current is applied between the electro-
des, which circulates through the orifice, where it is
carried by incoming liquid metal. The presence of
Industrial Engineering Program, Mechanical Engineering Department, particles in the liquid flow modifies the electrical
College of Engineering, Salman bin Abdulaziz University, AlKharj, Saudi resistance detected at the orifice. The change in
Arabia resistance causes a voltage pulse of duration approxi-
*Corresponding author, email [Link]@[Link] mately equal to the transit time it takes the particles to

ß 2013 W. S. Maney & Son Ltd.

Received 17 February 2013; accepted 27 June 2013
296 DOI 10.1179/1743133613Y.0000000070 International Journal of Cast Metals Research 2013 VOL 26 NO 5
 Al Kahtani Inclusion measurements in Al–6Si alloys

appear across the orifice. The voltage drop across the Experimental
orifice is monitored. The signal processing system
translates the voltage fluctuations and the distribution Commercial pure aluminium (99?78% purity) and
of their amplitudes to particles, and the volume experimental Al–6Si alloy were used in the present
distribution of these particles is expressed in the form work. Various inclusion additions were made to their
of histograms, showing the particle density per particle melts as follows:
size interval. (i) inclusions of Al4C3, CaO and MgO were added
The LiMCA analyser provides continuous online in the form of powder
measurements of the number of inclusions (expressed (ii) inclusions of Al2O3 were added in the form of
in thousands per kilogram, ‘K/kg’) up to 300 mm an Al–Al2O3 metal matrix composite alloy
diameter. These data can be analysed as total counts. (iii) inclusions of TiAl3 added in the form of Al–
In addition, the qualitative information concerning the 10Ti master alloy (waffles)
nature and species of the inclusions is very valuable in (iv) in addition to the powder form, TiB2 was also
the study and understanding of their sources. The added in the form of Al–5Ti–1B master alloy
impact of furnace preparation, alloying practice, feed (waffles).
stock mix, settling time and similar parameters on melt Individual powder injections were made to 2 kg melts of
cleanliness can be determined, allowing the development pure aluminium (or Al–6Si alloy) using a special powder
of process practices and procedures to minimise or injection apparatus as described in Ref. 7. The melting
eliminate their occurrence as claimed by the apparatus (pure Al or Al–6Si alloy) was carried out using an
manufacturer.6 electric resistance furnace in 2 kg silicon carbide
The present study was undertaken to investigate the crucibles. The temperature of the melt was kept at
capability of the LiMCA technique for measuring ,750uC. Degassing was carried out before injection
different types of inclusions in pure aluminium and an using pure, dry argon for ,15 min, after which
experimental Al–6Si casting alloys at 680uC melt skimming of the surface dross was carried out. The
temperature. The main propose was to evaluate the powder was injected into the degassed metal and
technique in the case of casting alloys, where the mechanically stirred to insure uniform distribution of
inclusion levels are considerably higher than those found the powder throughout the molten metal. The melt was
in wrought aluminium alloys for which the LiMCA has thereafter poured in a rectangular metallic mould
generally been used to date. It should be born in mind (266610 in) to produce blocks rich in a certain type
that the inclusions used in the present study may have of inclusion. These blocks were used to introduce
been affected by the methods of introduction and, inclusions into an 18 kg molten metal (pure aluminium
hence, not necessarily those that exist in commercial or Al–6Si) that was previously degassed for 30 min using
alloys. pure argon to remove the pre-existing inclusions. The

Table 1 Summary of different types of inclusions observed in molten aluminium1,2

Type Morphology Size range/mm

Oxides
Al2MgO4 (spinel) Al2O3 (corundum) Particles, skins, flakes 1–6
MgO, SiO2, CaO Particles, skins, films 10–1000
Polygonal particles, skins 0.2–1
Lumps 0.5–5
Particles ,5
Carbides
SiC Particles 0.5–25
Al4C3 Rectangular or hexagonal disc 0.5–25
Borides
TiB2 Clusters of hexagonal or rectangular discs 1–50
AlB2 Particles, clusters 1–20
VB2 Clusters 1–20
ZrB2 Particles, discs 1–10
Nitrides
AlN Particles, clusters 10–50
Other
Chlorides and salts Liquid droplets 0.5–1
(CaCl2, NaCl, MgCl2)
Flourites (cryolite)
Sludge Al(FeMnCr)Si
Calcium silicate Lumps or sphere-like particles 10–100
Potassium silicate Lumps or sphere-like particles 1–1000
CaSO4 Rods 1–5
Na3AlF6 Spheres 2–60
Ultrafine gas bubbles 10–30
Argon bubbles
N2 bubbles
Intermetallics
TiAl3, TiAl, NiAl, NiAl, Al3Zr Particles, clusters 10–100

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Al Kahtani Inclusion measurements in Al–6Si alloys

1 Schematic representation of inclusion addition procedure

chemical analysis and sizes of the used powders are In order to obtain a qualitative understanding of the
given in Table 1. LiMCA data acquired for different inclusion additions
A schematic representation of the inclusion addition to the pure aluminium and Al–6Si alloy melts, metallo-
and LiMCA sampling procedure is shown in Fig. 1 for graphy samples for microstructural analysis were pre-
the addition of a certain type of inclusions as an pared from the solidified metal in the LiMCA probe
example. It is to be mentioned here that each LiMCA tube resulting after a particular LiMCA data acquisi-
sampling was performed over a period of 30 min, and tion. Figure 2a shows examples of LiMCA tubes before
readings were taken at every 1–2 min intervals. In some and after sampling, while Fig. 2b shows a close up of the
cases, the sampling line was extended to 40 or 50 min to actual solidified metal block obtained from within the
determine if any changes occurred in the stable level of probe tube. In this case, the sample was sectioned from
the inclusion readings after the 30 min period. the solidified block of metal, mounted in bakelite and
After connecting the LiMCA to the microcomputer, polished to a fine finish (1 mm diamond paste). Figure 2c
the argon and air flow valves are opened (at 50–60 and shows clearly how the sectioning was carried out and the
75–80 lb in22 pressures respectively), after which the tube mounted sample. It should be noted that there is an
is inserted in the probe head section. The support pressure initial period of about 15–20 min before the inclusion
of the system appears on the system status page as readings begin to be detected properly by the LiMCA
28?6 lb in22. The pressure in the probe tube is supposed machine.
to vary between 2?5 and 22?5 lb in22 (vacuum). After the Besides the LiMCA probe tube samples, metallogra-
pressure/vacuum (Pres/Vac) value appears on the config- phy samples were also prepared from samplings taken
uration page, the calibration is carried out using the from the melts before and after the LiMCA test was
automatic control panel. After calibration, six bars carried out. These samplings were poured into a small
appear in the form of a histogram. They must be of metallic cup and allowed to solidify. In each case, a
equal height with a noise level lower than six. sample was then sectioned from the central part of the
After this step, the melt surface is carefully skimmed casting (20620 mm in size, 5 mm thick). The sectioned
to remove any dross and oxide layers. Then the LiMCA piece was mounted in bakelite and polished to a fine
head is inserted 1 in inside the melt and is kept as such finish, as before. An optical microscope-Clemex image
until the temperature of the thermocouple reaches 200uC analyser system was employed to examine the different
in order to preheat the tube. The tube, made from inclusion types observed in the various samples. In
alumina silicate, is sensitive to thermal shock. The certain cases, electron probe microanalysis (Jeol model
pressure of the tube is set to 2?5 lb in22 in manual set-up JXA-8900R, operating at 20 kV and 30 nA, with an
mode in order to avoid the entering of the metal into the electron beam size of y1 mm) was also used to
tube while the head is immersed in the melt. Later on, complement the analysis and to confirm the composition
when the tube is inside the molten metal, the set-up of inclusions observed in the microstructure, using
pressure mode is changed to automatic. The cycle time, wavelength dispersive spectroscopy and energy disper-
which is the time during which the metal comes in and sive X-ray (EDX) analysis. In some cases, X-ray
goes down the tube, is typically set to 40 s. In each cycle, elemental mapping/imaging was also employed.
including vacuum, acquisition and pressure, the data This study highlights some of the more interesting
corresponding to one sampling are displayed on the data obtained from the various LiMCA samplings. It
microcomputer screen in the form of an X–Y plot of the ought to be mentioned that most of the micrographs
total number of inclusions as a function of time. presented here were obtained from alloy melts at 680uC

298 International Journal of Cast Metals Research 2013 VOL 26 NO 5

 Al Kahtani Inclusion measurements in Al–6Si alloys

2 a liquid metal cleanliness analyser tube before and after sampling, b close up of actual solidified metal block obtained
from probe tube and c sectioned and mounted sample

melt temperature to minimise any possibility of floata- for ,30 min. The second CaO inclusion containing ingot
tion/sedimentation of the inclusions. was added, and the same procedure was repeated,
followed by the third addition and the correspond-
Results and discussion ing LiMCA sampling. The primary size of the CaO
powder particles used for injection was ,10 mm (Table 2).
Given that the emphasis of this study is more on Figure 3 compares the concentration number of inclusions
inclusions in the Al–6Si alloy, the microstructures shown in pure aluminium with those in the CaO containing melt,
in this section mainly cover the Al–6Si alloy samples. as a function of time. After 20 min of testing, most of the
Some examples of inclusions added to commercial pure inclusions settle to the bottom of the crucible. The
aluminium have also been provided. CaO inclusions decrease from their initial level of
Inclusions in pure aluminium melts
The addition of CaO inclusions to a pure aluminium melt
was carried out using prefabricated CaO inclusion
containing aluminium ingots. As described previously,
the inclusion addition was carried out in three stages. After
the first addition, the melt was stirred properly, followed
by a LiMCA sampling that was continued without pause

Table 2 List of inclusions used in present work

Type Chemical analysis/ wt-% Powder size/mm

a-Al2O3 Al2O3599 y20

MgO MgO596 min y70
CaO CaO599 y10 3 concentration number of inclusions in commercial
TiB2 TiB2599 y2–5 pure aluminium as a function of time when CaO was
Al4C3 Al4C3599 y10
added

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Al Kahtani Inclusion measurements in Al–6Si alloys

4 a backscattered electron images of CaO inclusions and b X-ray image of Ca

147–6?1K kg21, while in commercial pure aluminium, the inclusion containing aluminium ingot. Figure 5a shows
level of inclusions decreases from 54?5 to 2?8K kg21, the plot of the concentration of inclusions versus time.
reaching the minimum within 20 min only. Figure 4 shows In each sampling, the concentration of inclusions
an example of (a) the backscattered electron image of CaO dropped gradually after 20 min to its lowest level. In
inclusions observed in a commercial pure aluminium addition, the highest levels of inclusions were detected in
sample obtained from the LiMCA probe tube at the the 20–25 mm particle size range.
beginning of the LiMCA testing, and (b) the correspond- Figure 5b shows an example of two MgO inclusion
ing X-ray image of Ca. In this figure, a cluster of these particles in the aluminium matrix of a sample obtained
inclusion particles is seen in conjunction with black pores from the LiMCA probe tube. Compared to the MgO
in the vicinity of the inclusions (white arrows). particles shown in Fig. 5b, Fig. 6a exhibits an example
The addition of MgO inclusions to the pure alumi- of MgO inclusions occurring in the form of oxide films
nium melt was carried out using the prefabricated MgO within shrinkage pores in the aluminium matrix,

5 a concentration number of inclusions in commercial pure aluminium as function of time when MgO was added and
b backscattered electron image of two MgO inclusions in commercial pure Al matrix

6 a backscattered electron image showing example of MgO films in commercial pure Al, obtained at the start of a
LiMCA test and b corresponding X-ray image of oxygen

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 Al Kahtani Inclusion measurements in Al–6Si alloys

7 a concentration of inclusions in commercial pure aluminium as a function of time when TiAl3 was added and b back-
scattered electron image of TiAl3 size and distribution in pure aluminium

corresponding to the LiMCA probe tube sample taken The efficiency of the Al–Ti master alloy would thus vary,
at the beginning of the LiMCA test, after the addition of depending on the relative amounts of these long plates
Mg metal to the MgO inclusion containing Al melt and versus the very small particles of TiAl3 present in the
its subsequent oxidation. The black lace-like features master alloy. This would explain the inconsistent
observed in the region indicate that these are oxide films. behaviour reported for Al–Ti master alloys and why
As can be seen, the oxide films are associated with they are less effective than Al–Ti–B master alloys.8,9
porosity. The corresponding oxygen image is shown in Inclusion in Al–6Si alloy ingots
Fig. 6b, confirming that these were oxide films.
The addition of Al4C3, CaO and MgO inclusions to the
Figure 7a shows the concentrations of TiAl3 inclu-
Al–6Si alloy melt were carried out using prefabricated
sions versus time. The number of inclusions shows no
Al4C3 inclusion containing Al–6Si alloy ingots, whereas
abrupt drop in level after 30 min. It is worth nothing
TiB2 was added as Al–5Ti–1B master alloy.
that, in this case, the volume of TiAl3 inclusions remains
Figure 8 shows the distribution of Al4C3inclusions as
comparatively high in all particle size ranges, whereas in
a function of time. The LiMCA measures the increase in
the case of other inclusions, the higher particle size
inclusion concentrations with respect to the base alloy
ranges showed low concentrations. Figure 7b is a
backscattered electron image of TiAl3 inclusions in
commercial pure Al obtained from a sample taken at the
start of the LiMCA test. The TiAl3 inclusions were
added to the pure Al melt in the form of Al–10Ti master
alloy waffle. The inclusions are observed in the form of
fine bright white particles in the matrix, and the X-ray
images of Ti confirmed that they are TiAl3 inclusions.
Such small inclusions are responsible for the grain
refining properties of the Al–10Ti master alloy.8
However, the majority of TiAl3 particles in the master
alloy used appear in the form of plates of considerable
lengths. These particles, being much larger than the
grain sizes observed in the Al–Si alloy samples to which
the Al–10Ti master alloy was added, are obviously not
expected to act as nucleants for the solidifying alumi- 9 Concentration numbers of inclusions in Al–6Si alloy as
nium (and hence take part in the grain refining process). function of time when CaO was added

8 Concentration numbers of inclusions in Al–6Si alloy as 10 Concentration numbers of inclusions in Al–6Si alloy
a function of time when Al4C3 is added as a function of time when MgO was added

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Al Kahtani Inclusion measurements in Al–6Si alloys

the inclusion levels were sufficiently high to allow

detection from the start of the sampling period. The
total number of CaO inclusions measured over 60 min
of LiMCA sampling is illustrated in Fig. 9. As can be
seen, the curves are similar in the four cases: the CaO
inclusion containing Al–6Si melts display almost double
the concentration of inclusions at the start of sampling;
the concentrations decrease at similar rates until a
steady state is reached after about 35–40 min of
sampling time, when all four melt conditions (including
the base alloy melt without CaO inclusion addition)
show a very low level of inclusions, indicating that the
inclusions have settled to the bottom of the melt
11 Concentration numbers of inclusions in Al–6Si alloy crucible. Figure 10 is showing the total number of
as a function of time when TiB2 was added MgO inclusions over the 60 min period of LiMCA
sampling. All curves show similar trends. The inclusion
levels drop within 20 min of the testing period and then
gradually reach low, steady state levels. Surprisingly, the
Al–6Si base alloy melt shows higher inclusion levels than
those observed after the first MgO addition until they
reach their steady state level after ,40 min of sampling.
The variation in the total number of TiB2 inclusions
as a function of time is illustrated in Fig. 11. As can be
seen, the inclusion concentration increases with addition
of the TiB2 inclusion containing ingot. With further
additions, the inclusion concentrations decrease some-
what. However, each curve follows the same decreasing
trend, and stabilisation is achieved after ,45 or 50 min
of testing, due to settling of the TiB2 inclusions (density
of 4?5–4?6 g cm23) to the crucible bottom. The TiB2
12 Concentration numbers of inclusions in Al–6Si alloy
particles possess excellent wettability with respect to
as a function of time when Al2O3 was added (MMC liquid aluminium facilitating their injection into the
source) melt. This is reflected by the similarity of the four curves
seen in the plot where, with reference to the base alloy
curve, the increase in inclusion levels with TiB2 additions
melt, and the levels become negligible after ,40 min of shows corresponding displacements in the other three
testing. As can be seen, the first and second additions curves.
show only a slight increase with respect to the base alloy Figure 12 shows the LiMCA samplings corresponding
melt readings. With the third Al4C3 inclusion addition, to the Al2O3 inclusion addition. The source of Al2O3

a Al4C3; b CaO; c MgO; d TiB2

13 Optical micrographs showing inclusions observed in Al–6Si alloy

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 Al Kahtani Inclusion measurements in Al–6Si alloys

regions. Similarly, the CaO inclusions in Fig. 13b appear

as clusters (bumpy looking areas) in the Al–Si eutectic
regions, with lighter grey polygonal particles (compared
to the darker colour of the Si particles) occurring close
to them. In comparison, the large agglomerate of MgO
inclusions in Fig. 13c makes it difficult to pinpoint the
matrix region.
However, the a-Al dendrite contours on the upper
right side indicate that the inclusions are probably
located within a pore in the matrix. The main point of
interest to note is that the TiB2 inclusions in Fig. 13d are
present in very large amounts compared to the other
inclusions. They also appear to be located over porous
14 Backscattered electron image of TiAl3 inclusions in areas (dark regions interspersed between the TiB2
Al–6Si alloy particles) in the Al–Si interdendritic regions and also
within the a-Al dendrites to a small extent.
inclusions was in the form of an Al–20 vol.-%Al2O3 Figure 14 reveals the presence of TiAl3 inclusions in
particulate reinforced aluminium metal matrix compo- Al–6Si alloy melt obtained from the LiMCA probe tube
site alloy. In general, due to the density difference at the start of a LiMCA test. It ought to be mentioned
between the Al2O3 inclusions and the melt, the inclusion here that a LiMCA probe tube sample obtained ‘‘at the
concentrations drop considerably after 10–15 min of start’’ of a LiMCA test means that the probe tube was
sampling, then decrease gradually and remain stable removed from the melt after ,2 min of the LiMCA
after ,25 min. sampling. The melt was stirred again to ensure homo-
Examples of Al4C3, CaO, MgO and TiB2 inclusions geneous distribution of the inclusions, and a new
observed in the optical micrographs of samples taken LiMCA test started, using a fresh probe tube. The
from the respective inclusion containing Al–6Si alloy solidified metal in the first probe tube was sectioned to
ingots are shown in Fig. 13. All micrographs are taken produce the metallography sample corresponding to the
at the same magnification of 6200. One of the ‘start of LiMCA test’ conditions.
interesting features to note in these micrographs is that Figure 15 represents the TiAl3 inclusions observed in
the inclusion particles are often associated with pores in the form of long (Fig. 15a) and short (Fig. 15d) plates,
their vicinity. The Al4C3 inclusions in Fig. 13a are the taken respectively, from LiMCA probe tube samples
small black particles scattered in the Al–Si eutectic obtained at the start and end of a LiMCA test. The

15 Backscattered electron images showing a, d long and short TiAl3 plates and corresponding images of b, e Ti, c Si
and f Fe; samples obtained from LiMCA probe tube at a–c start and d–f end of LiMCA test

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Al Kahtani Inclusion measurements in Al–6Si alloys

16 Optical micrographs showing massive sizes and acicular nature of TiAl3 inclusion particles (arrowed) in Al–6Si alloy
melt to which Al–10Ti master alloy was added

17 a backscattered electron image of CaO inclusions and Ca containing compounds in Al–6Si alloy and b oxygen distri-
bution in black areas in a and c corresponding EDX spectrum

18 a backscattered electron image of Al4C3 inclusions (arrowed) in Al–6Si alloy mixed with oxide films and b corre-
sponding X-ray image of carbon

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 Al Kahtani Inclusion measurements in Al–6Si alloys

19 Optical micrographs showing Al4C3 inclusions in Al–6Si alloy samples a before start and b at end of LiMCA test

variation in length of the TiAl3 particles is brought out machining problems. With reference to the LiMCA
clearly if we consider the magnifications at which these test, obviously, TiAl3 plates of such large size will be
the two backscattered electron images were taken (6800 inhibited from entering the probe tube orifice (of
and 62500 respectively). The X-ray images of Ti 300 mm diameter).
(Fig. 15b) for the two backscattered electron images Figure 17a is a backscattered electron image taken
confirms that these are Ti containing particles. The X- from an Al–6Si alloy melt to which CaO inclusions were
ray image of Si (Fig. 15c), corresponding to the BE added. The metallography sample in this case was
image in Fig. 15a, reveals the distribution of the silicon obtained from the sampling cup casting taken from the
particles in the Al–Si eutectic regions and which are melt before the LiMCA test was started. The micro-
observed as pale grey constituents in Fig. 15a. structure reveals faint Al–Si eutectic regions towards the
In addition, it is also noticed that the TiAl3 plates/ top left of the figure, bright irregular shaped particles
particles contain some Si as well. Thus, these particles and black clusters associated with the latter. From the
would correspond more correctly to (Al,Si)3Ti rather EDX spectrum (Fig. 17c) of the bright particles, it
than TiAl3. In Fig. 15d, a couple of b-Al5FeSi iron would be reasonable to conclude that these particles are
intermetallic plate-like particles are also observed, Ca containing compounds that have formed as a result
associated with the TiAl3 plates, and the corresponding of the reaction between the CaO inclusions and the melt.
X-ray image of Fe shown in Fig. 15f points clearly to With respect to the X-ray image of oxygen shown in
their location in the matrix. As mentioned previously in Fig. 17b, and comparing it with the backscattered
the context of grain refining, it is the very small electron image in Fig. 17a, the bright patch on the
(Al,Si)3Ti particles such as those shown in Fig. 15d that upper right would most probably correspond to an
more likely act as nuclei for the nucleation and growth oxide film within the black, elongated pore observed in
of the a-Al dendrites rather than the large (Al,Si)3 Ti the backscattered electron image. In comparison, the
plates of Fig. 15a. bright particles along the left bottom of the elongated
The optical micrographs of Fig. 16 show the acicular pore in Fig. 17a are more likely Ca containing
morphology of the TiAl3 plates in Al–6Si alloy, compounds rather than CaO.
obtained from the addition of Al–10Ti master alloy In a study on the role of inclusions in nucleating a-Al
to the melt and taken from a LiMCA probe tube and Fe intermetallics in the Al rich corner of the Al–Si–
sample at the start of the LiMCA test. The large plates Fe ternary system, Khalifa et al.7 reported that the CaO
are the ones that act as deleterious inclusions and have particles interact with the aluminium alloy melt to form
little or no contribution towards grain refining. The Ca compounds rich in silicon due to the high chemical
presence of these hard, acicular plates is actually affinity of CaO to form intermetallic compounds with
harmful to the casting in terms of tool wear associated Al–Si melts. The present findings also confirm these

20 Optical micrographs showing MgO inclusions in Al–6Si alloy samples a before start and b at end of LiMCA test

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Al Kahtani Inclusion measurements in Al–6Si alloys

21 Optical micrographs showing Al2O3 inclusions (arrowed) in Al–6Si base alloy, obtained from casting samples taken at
a start and b end of LiMCA measurement

results, as seen from the EDX spectrum of Fig. 17c, reacted with the melt. Probably on account of their size
where peaks for Al, Si and Ca are clearly observed. and morphology, the Al2O3 inclusions appear in loosely
The backscattered electron image of Fig. 18a reveals grouped entities within the matrix, in the Al–Si eutectic
the presence of several particles within the matrix, taken regions. The backscattered electron image of TiB2
from a sampling cup casting of the Al4C3 inclusion particles in Al–6Si alloy is shown in Fig. 22a where, in
containing Al–6Si melt before starting the LiMCA test. this case, the TiB2 inclusions were added in the form of
The X-ray image of carbon distribution is shown in Al–5Ti–1B master alloy. The matrix exhibits TiB2
Fig. 18b, indicating that these constituents are, in fact, a particle clusters in the centre and upper half of the
mixture of oxides and carbides particles, where the image, along with large dark grey particles of unde-
carbide particles are those arrowed in Fig. 18a. The composed master alloy. Some oxide films are also
optical micrographs of Fig. 19, obtained from the same observed. The corresponding X-ray images (Fig. 22b
sample as well as a casting sample obtained at the end of and c) of Ti and B respectively distinguish the locations
the LiMCA test, show how the Al4C3 inclusions actually of the TiB2 inclusions from the oxide films.
appear in the matrix. It is noticed from this figure that An excellent example of the agglomeration of TiB2
there are much larger concentrations of Al4C3 in the inclusions as captured by the LiMCA probe tube is
samples at the start, compared to those obtained at the shown in Fig. 23a. Note the vast amount of TiB2
end of the test. In addition, the inclusions appear to be particles that constitute the agglomerate. The corre-
generally associated with oxide films judging by the lace- sponding X-ray images of Ti and B in Fig. 23b and c
like features of the regions in which they are found. The confirm that these are TiB2 inclusions. It should be
optical micrographs of Fig. 20 provide examples of noted that due to the difficulty associated with mapping
MgO inclusions (powder addition) in Al–6Si alloy, taken boron, the X-ray map for B is rather faint compared to
from a sample obtained from the corresponding melt that of Ti. Nevertheless, the contour of the agglomerate
before the start of the LiMCA test (Fig. 20a) and after can still be distinguished in Fig. 23c. The results
the LiMCA test (Fig. 20b). presented in Fig. 23 constitute a very important aspect
Examples of Al2O3 inclusions observed in Al–6Si of the LiMCA.
alloy melts are shown in Fig. 21. The Al2O3 inclusions Other melt cleanliness techniques such as Prefil10 and
were added in the form of an Al–Si–Mg/Al2O3/10p PoDFA11 cannot measure such clusters or agglomerates
metal matrix composite. As reported previously, these of TiB2 inclusions, as the filters in these systems
inclusions have particle sizes ranging from 4 to 60 mm, invariably become blocked, interrupting/stopping the
the average particle size being y23 mm. The rough measurements. The LiMCA, on the other hand, is able
contours of the particles indicate that these particles to capture these clusters without any problem.12 The

22 a backscattered electron image showing TiB2 inclusions tangled with oxide films resulting from Al–5Ti–1B master
alloy addition to Al–6Si alloy and b, c corresponding X-ray images of Ti and B respectively

306 International Journal of Cast Metals Research 2013 VOL 26 NO 5

 Al Kahtani Inclusion measurements in Al–6Si alloys

23 a backscattered electron image showing large agglomerate of TiB2 inclusions resulting from Al–5Ti–1B master alloy
addition to Al–6 alloy, obtained from sample taken from LiMCA sampling probe at start of LiMCA test and b, c corre-
sponding X-ray images of Ti and B respectively

only limitation for the LiMCA would be that posed by References

the size of the probe tube orifice. Thus, it appears that
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the LiMCA technique is the only means to measure TiB2
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1. The LiMCA could successfully be used to measure 5. M. H. Mulazimogolu, N. Handiak and J. E Gruzleski: ‘Some
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measurement that is consistent with approximate tion of modified A356 alloy’, AFS Trans., 1989, 97, 225–232.
quantity of precipitate added; the accuracy is not 6. ‘LiMCA II operation and maintenance guide’, Version 2-0, Bomem
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Gudmundsson and D. Bristow: ‘Studies on the dissolution of Al–
the surrounding molten alloy to form a complex
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It depends mainly on the amount of added inclusions, 11. D. Doutre, B. Gariepy, J. P. Martin and G. Dube: ‘Aluminium
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the added inclusions. Met., 1994, 915–920.
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Acknowledgement molten metal processing on mechanical properties of cast Al–Si–
Mg alloys’, AFS Trans., 1989, 97, 811–823.
The author would like to thank Professor F. H. Samuel 14. M. M. Gusoweski, G. K. Sigworth and D. A. Senter: ‘‘The role of
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of the Université du Québec à Chicoutimi for his Trans. A, 1987, 18A, 603–619.
technical help and support during the course of the 15. G. K. Sigworth and M. M. Gusoweski: ‘‘Grain refining of
experimental work. hypoeutectic Al–Si alloys’, AFS Trans., 1985, 93, 907–912.

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