Method Developed for Quantitative Analysis of Inclusions

in Solidified Aluminum Ingots

MAJED M. JARADEH and TORBJORN CARLBERG

A deep-etching method was used to determine inclusions in solidified direct chill cast aluminum
ingots. The technique was developed to allow easy quantification of the amount and size dis-
tribution of inclusions over billet lengths and cross sections. A pressure filtration (Prefil) test
also was used to verify molten alloy cleanliness during casting, and the results of these mea-
surements then were compared. The amount and distribution of nonmetallic inclusions were
analyzed, as determined using a NaOH deep-etching method over billet lengths and cross
sections. A higher inclusion count was observed at both billet ends, with more inclusions located
nearer the billet section centerline. Furthermore, the inclusion density in the radial direction
at every distance along the billet length was distributed inhomogeneously. Differences were
observed between Prefil samples taken at different casting stages. The Prefil curves and metal-
lographic analysis of Prefil residue obtained from melt samples, at an early casting stage or
before degassing, indicate more oxides than in a melt sample taken under steady-state casting
conditions. A reasonable correlation was established between the number of inclusions in the
molten alloy (measured using Prefil and LiMCA) and the etch pits on deep-etched surfaces of
billet cross sections.

DOI: 10.1007/s11663-010-9463-4
Ó The Minerals, Metals & Materials Society and ASM International 2010

I. INTRODUCTION advantage of providing in situ results in the form of

THE term ‘‘inclusion’’ refers to any type of undis-
solved foreign material present in cast metal.[1] Inclu-
sions are well known as a common defect in cast
structures and normally are obtained during production
processes. The types, sizes, and sources of inclusions
present in aluminum, as well as their detrimental effects
on final products, have been reviewed in detail elsewhere
in the literature.[2–6]
Investigation of inclusions in aluminum alloys has
highlighted the importance of controlling their amount
and distribution during the production process. This
also has created the need for the ongoing development
and use of several melt treatment techniques, such as
SNIF,[7,8] as well as inclusion assessment methods. The
literature discusses many techniques for counting inclu-
sions in aluminum[3,9–13]; the LiMCA, PoDFA, and
LAIS techniques commonly are used, as is the pressure
filtration (Prefil) technique commercially known as the
Prefil-Footprinter.[14–19] The Prefil apparatus is one of
the more recent techniques used to determine the clean-
liness of liquid aluminum alloys. It measures the relative
cleanliness of a melt by comparison with the bench-
mark inclusion level for a given alloy, production
process, or stage in the process. This technique has the
advantage of flexibility, allowing inclusion measure-
ment at any stage of the process chain.[17] It also has the
MAJED M. JARADEH, Doctor, and TORBJORN CARLBERG,
Professor, are with the Department of Natural Sciences, Engineer-
ing and Mathematics, Mid Sweden University, FSCN, SE-85170
Sundsvall, Sweden. Contact e-mail: torbjorn.carlberg@miun.se
Manuscript submitted August 8, 2010.
Article published online December 15, 2010.
flow-rate charts. These charts minimize the need for the
time-consuming metallographic examinations of inclu-
sions demanded by other Prefil techniques, such as
PoDFA and LAIS.
All aforementioned inclusion assessment techniques
are used on the molten aluminum and are expensive or
time consuming. Assessment using prefiltration tech-
niques as (PoDFA, LAIS, and Prefil) involves concen-
trating the inclusions, which means that some
information is lost (e.g., as inclusion distribution within
the metal). Because concentration also involves some
degree of agglomeration, information about inclusion
size and shape also might be lost.[10] When it comes to
assessing inclusions in the solidified product (i.e., after
being cast), only a few inclusion assessment methods are
known and supporting literature data are lacking. A
typical inclusion assessment method is the light micros-
copy examination of metallographically prepared sam-
ples. Obtaining results by this method, however, is time
consuming. As a result of the low inclusion contents and
the high tendency of inclusions to segregate into a
nonuniform distribution, the direct microscopic analysis
of a metal sample surface is impractical because a large
area would have to be observed for quantitative
assessment.[10]
The present work has developed a simpler test for
inclusion assessment in solidified aluminum castings,
using an NaOH deep-etching technique.[20] One reason
for using the deep-etching method concerns the random
occurrence of inclusions in Al ingots; another reason
concerns the difficulty of applying the available detec-
tion and quantitative assessment techniques. Further-
more, the actual distribution of inclusions in final

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 42B, FEBRUARY 2011—121

castings should be known, not only their occurrence in
the melt, which is possible with the new technique.
The work aims to develop deep-etching into a
quantitative analysis technique for determining alumi-
num casting quality and then correlating ingot quality
with melt quality, as measured using the Prefil or
LiMCA techniques. In this first benchmark study using
the deep-etching technique, only a few examples of what
can be studied have been investigated. Additional
studies will explore how to influence the inclusion
distribution, in which context the new technique will
be an important diagnostic tool.
II. EXPERIMENTAL PROCEDURES
A. Materials and Sample Preparation
Direct chill (DC)-cast billets of extruded AA 6063
aluminum alloy containing 0.5 wt pct Si and 0.45 wt pct
Mg were analyzed for inclusions in the present study.
The alloy melts were refined by degassing (SNIF)[8]
before casting.
The billets were 152 and 228 mm in diameter. Cross-
sectional slices of the billet were cut in transverse
direction at various locations along the billet length
from bottom to top. To quantify inclusion distribution
in the radial direction, each cross-section billet slice was
divided into the following zones of equal area: surface
(S), midradius (MR), and center (C). In addition, six
radial positions were selected on each. Details of the
sampling are depicted schematically in Figure 1.
B. Assessment Methods
1. Deep-etching test
The deep-etching test was used to evaluate inclusions
in solid aluminum castings. This test used a solution of
10 to 20 g of sodium hydroxide (NaOH) in 100 mL of
water at 333 K to 343 K (60 °C to 70 °C) for 5 to
15 minutes of etch time.[21] After etching by immersion,
the etched slices were washed with water. The surface
usually was scrubbed thoroughly with a brush to remove
any smut that could mask the etched surface. The
surface conditions for parts to be deep etched are not
critical, as any flat ground surface obtained using a
turning machine is adequate. However, the surface
should be free of grease or oil to permit even etching.
The deep etching dissolves out the inclusions, gener-
ating etch pits (holes) on the surface that can be
observed by the naked eye. To characterize the inclusion
distribution easily in billet slices, the etched surfaces
were mapped using a normal copy machine, and the
copies then were scanned to a computer. The inclusions
that become visible as black dots then could be counted,
regardless of the pit type, visually or by using an image
analysis program. Thus, information on inclusion size
distribution, along the whole billet, can be acquired.
2. Prefil-footprinter test
The Prefil technique was used to assess the quality of
the studied molten alloy during the casting process. The
122—VOLUME 42B, FEBRUARY 2011
Prefil apparatus and the operating principle[16] are
outlined in Figure 2. A sample of the molten alloy is
poured into a preheated crucible through a fine porous
filter disc at constant temperature and pressure. The
amount of metal filtered is recorded using a digital
balance, yielding a graph of weight filtered vs time.
Inclusions in the melt quickly build up on the surface of
the test filter, reducing the rate of flow through the filter.
The slope and overall shape of the flow rate curve
indicate the level of inclusions present in the melt; the
cleaner the melt, the faster it will flow through the filter
and the higher the slope of the resulting curve.[15]
The following Prefil samples were taken during the
casting operation from a melt: after degassing at times
corresponding to billet lengths of 1.6 m (test 1) and 4 m
(test 2) as well as before degassing (test 3). After each
test, the solidified metal above the filter was sectioned,
mounted, and polished for metallographic examination.
C. Metallographic Examination
Metallographic analysis was used to allow identifica-
tion and quantification of the types of inclusions present
in the alloy samples. It involved examining both selected
15 9 10-mm2 pieces cut from the studied deep-etched
slices and unfiltered metal residue captured at the
surface of the Prefil filter. The polished samples then
were analyzed using an optical microscope and a
scanning electron microscope (SEM) equipped with an
energy-dispersive X-ray (EDX) spectrometer. In Prefil
samples, inclusion counting was done using the grid
method[15] based on the PoDFA technique (i.e., the total
inclusion area is obtained and then divided by the
weight of the metal that has passed through the filter
[mm2 kg–1]). In the samples cut from the deep-etched
slices, a 0.3-mm-thick surface layer was removed by
grinding to enable the inclusions to be observed through
an optical microscope after the acid etching.
III. RESULTS
A. Evaluation of Billet Quality
1. Deep-etching results
The optical micrographs presented in Figure 3 show
how an inclusion develops through several etching steps
into a large etch pit visible under low magnification or to
the naked eye. It is clear that the inclusion initiated the
hole and that the AlFeSi phases in the area reacted
differently from the inclusions. Figure 3(a) follows the
etching of a TiB2 cluster, and Figures 3(b) and (c) show
that Al2O3 film, MgO, and MgAl2O4 inclusions also
behaved in the same way. An undissolved Al3Ti particle
and an Al6(Fe,Mn) particle also were examined but did
not produce etch pits. The diameters of pores also
increased after deep etching, forming holes visible to the
naked eye.
From the optical images in Figure 3, one also can
observe that the size (i.e., mean diameter) of the pit after
15 minutes of etching is approximately ten times larger
than the size of the TiB2 cluster before etching.
METALLURGICAL AND MATERIALS TRANSACTIONS B
Fig. 1—A schematic of sampling positions: (a) sectioning along the length of a DC-cast billet; (b) the positions of zones for measuring the radial
distributions.
B. Inclusion Amount and Size Distribution
Figure 4 shows typical macroscopic views of inclusion
distributions on deep-etched cross sections of a 152-mm-
diameter billet. The images are typical of the results
observed in several studied billets. They clearly exhibit a
nonuniform lateral distribution of etch pits (black dots)
at every billet height from bottom to top. It is clear that
both ends of the billet (i.e., first and last slices in
Figure 4) have more inclusions than do the slices in
between. It also is shown that the first slice at the
position 2.5 cm from the bottom block displays numer-
ous small holes—most of them under 0.1 mm2 in
METALLURGICAL AND MATERIALS TRANSACTIONS B
area—arranged in a circular zone near the surface or
mold wall.
If the billet cross section is divided into two equal
areas, indicated by dashed circles in Figure 4, then more
inclusions generally are shown in the billet’s outer
region.
Figure 5 shows a typical inclusion distribution pattern
along a billet length. Only pits of an area equal to or
larger than 0.05 mm2, clearly identifiable by the naked
eye, were counted. The most important trend in pit
location is that the number of pits is higher at the
bottom, low in the center, and increases slightly at the
VOLUME 42B, FEBRUARY 2011—123
Fig. 2—Prefil-Footprinter operation steps.[16]

Fig. 3—(a) Optical images of a TiB2 cluster after subsequent etching steps. (b) Optical images of Al2O3 oxide film after subsequent etching steps
(0-, 2-, 4-, and 13-min etch times). (c) Optical images of a spinel after subsequent etching steps (0-, 2-, 4-, and 13-min etch times).

top part of the billet. Most etch pits are located on the
bottom end of the billet (i.e., at the start of casting).
Figures 6(a) and (b) show deep-etched longitudinal
sections, taken from both ends of a 152-mm-diameter
billet (i.e., at the bottom [start of casting] and the top
[end of casting], respectively). These parts of a billet
often display the highest densities of etch pits (Figures 4
and 5). The images show many inclusions around the
billet central axis, indicated by a dashed line. The
bottom slice in Figure 6(a) also has a high density of
inclusions near the surface, similar to the transverse slice
at position 2.5 cm in Figure 4.
For the studied 228-mm-diameter billet, a visual
investigation of four slices, cut along the billet length,
revealed a macroscopic view of nonuniformly distrib-
uted inclusions, similar to that shown in Figure 4.
The etch pits were observed under an optical micro-
scope and were classified in terms of size. The pits were
approximately circular in shape and were classified
based on their mean diameter (dm). The following size

124—VOLUME 42B, FEBRUARY 2011 METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 4—Typical macroscopic view of billet cross sections, showing etch pits on deep-etched surfaces etched in 15 pct NaOH at 338 K (65 °C) for
12 min (slice positions are from bottom to top).
Fig. 5—A typical inclusion distribution along a 152-mm-diameter
billet after 12 min of etch time.
ranges were used: 0.2 < A < 0.3 mm, 0.3 < B <0.4 mm,
and C > 0.4 mm. The results of counting the inclusions
in these three size ranges are presented in Figure 7. It is
clear that many of the largest pits, C > 0.4 mm, were
located in the billet’s bottom portion. In contrast, in the
billet’s interior and top portions, small pits (i.e., class
0.2 < A < 0.3 mm) dominated.
The radial distribution of inclusions in the cross
sections of a 228-mm-diameter billet was investigated.
The etch pits were counted in C, MR, and S zones of
equal areas (Figure 1). The numbers of pits in each zone
relative to the total numbers in the whole cross section
(i.e., the percentage in each zone) are presented in
Figure 8. At every height along the billet length, the
higher inclusion population generally was found in the
center zone of the billet cross section. Figure 8 presents
a location comparison (i.e., center vs surface), indicating
significant differences along the billet length, with a
higher variation being observed in the populations in the
top portion of the billet.
METALLURGICAL AND MATERIALS TRANSACTIONS B
In Figure 9, inclusion counts at six radial cross-
section positions along a 228-mm-diameter billet are
plotted (Figure 1(b)). The most important trend in the
radial location of inclusions is their random distribution
throughout the billet cross section at the various
locations along the billet length. At approximately
0.2 m from the billet bottom, inclusions seem to
concentrate in two regions, peaking 65 mm from the
center line and 10 mm from the surface. At the
longitudinal positions corresponding to steady-state
casting (i.e., 1.6 and 4 m from the bottom), inclusions
are distributed more randomly but with a slightly lower
density at the surface. Near the top portion of the billet,
inclusion counts clearly peak in the center zone and
decrease toward the surface.
One also can observe that the distributions in two
sections near each other (i.e., 1.6 and 4 m from the
bottom) are parallel each other. These similarities,
which are also clear in the images in Figure 4, suggest
that radial distributions are not completely random and
that inclusion frequency varies periodically in the
casting system.
Optical and SEM/EDX microscopic examination of
inclusions in billet samples reveals TiB2 inclusions in the
form of clusters; Al4C3 inclusions in the form of
hexagonal platelets; as well as oxide particles and films
of Al2O3, MgO, and MgAl2O4 spinel. Figure 10(a)
shows the typical appearance of various types of
inclusions in the studied 6063 alloy.
Figures 10(b) and (c) present a comparison of the
dominant inclusion types in the slices taken from both
ends of a 152-mm-diameter billet (i.e., at start and end
of casting, respectively). It is obvious in Figure 10(b)
that TiB2 clusters dominate at the bottom, whereas
Figure 10(c) shows that oxide film agglomerations were
found in the top part of the billet. Figure 10(d) shows
VOLUME 42B, FEBRUARY 2011—125

Fig. 6—Deep-etched longitudinal sections cut from (a) the bottom
and (b) the top of a billet. The dashed lines indicate the billet central
axis, and the rectangular box shown by dotted lines indicates the
sectioning for metallographic analysis given in Fig. 10(d).
Fig. 7—The size distribution of inclusions along the length of a
228-mm-diameter billet.
126—VOLUME 42B, FEBRUARY 2011
various types of inclusions in the form of oxides coupled
to porosity that also were observed at the bottom of the
billet (indicated by an arrow in Figure 6(a)).
C. Evaluation of Melt Quality
1. Prefil results
The Prefil curves for filtration weight vs filtration time
at different test locations (i.e., from a melt that
corresponds to 1.6-m [test 1] and 4-m [test 2] billet
casting lengths) are presented in Figure 11. Different
slopes are observed (i.e., the curve was low in test 1 and
higher in test 2). This variation in the curvature of the
Prefil curve is associated with melt quality (i.e., the
presence of inclusions that gradually clog the filter and
reduce the filtration rate). Curve 1 represents a melt with
a considerable inclusion presence, and curve 2 represents
a melt with fewer inclusions. A Prefil curve of test 3,
which was taken before degassing, was not registered.
The Prefil samples were analyzed metallographically.
The inclusions, which were built up on the filter surface,
were examined using optical and SEM microscopy,
identified, and counted. The results are presented in
Table I, where the inclusion concentration is reported in
mm2 kg–1, indicating the area of inclusions in the
sectioned part per mass of filtered melt. Of the studied
Prefil samples, samples 1 and 3 were the dirtiest, with a
total inclusion content of 0.741 and 0.627 mm2 kg–1 and
32 and 33 oxide films per kilogram, respectively. Sample
2 was the cleanest, with an overall metal cleanliness of
0.234 mm2 kg–1 and 11 oxide films per kilogram.
Table I lists the total inclusions and oxide films as
measured in the Prefil analysis.
TiB2 was the main inclusion observed in the three
Prefil samples, accounting for approximately 80 to
90 pct of the total inclusions. All samples also contained
Al2O3 films, small and large Al4C3, MgO, and MgAl2O4
spinel. Figure 12 shows an example of TiB2 clusters
concentrated in the filter from Prefil test 1.
IV. DISCUSSION
A. The Assessment Methods
In this work, two assessment methods were used to
characterize inclusions in solid and liquid 6063 alumi-
num alloys produced by the DC casting process. The
advantages and disadvantages of these techniques are
discussed in the following sections.
1. Deep-etching method
The first question regarding the described deep-
etching method is whether the observed etch pits really
represent inclusions. The sequence of optical micro-
graphs in Figures 3(a) through (c) clearly shows how an
inclusion develops into a visible hole in the etched
surface. It is also clear that different phases, such as the
Fe- and Si-containing a and b phases and Al3Ti, do not
produce such reactions during deep etching. It seems to
be the nonmetallic foreign particles and not the inter-
mediate phases that react strongly during etching,
METALLURGICAL AND MATERIALS TRANSACTIONS B
Fig. 8—Radial distribution (pct of total number) of inclusions in three zones in 228-mm-diameter billet slices at four positions along a billet.

Fig. 9—Distribution of inclusions at six radial positions across 228-mm-diameter billet sections at four positions along a billet.

producing the desired effect. It is well known that NaOH
solutions strongly etch aluminum surfaces, and the
following reactions can occur[22]:
Al þ 3Na(OH) ! Al(OH)3 þ 3Na
2Al þ 2NaOH þ 6H2 O ! 2NaAl(OH)4 þ 3H2
2Al þ 2NaOH þ 2H2 O ! 2NaAlO2 þ 3H2
The surface is etched an average of approximately
0.3 mm during the deep-etching treatment; during the
treatment, pits form that are 10 times larger than the
inclusions, and these pits are in the order of 0.5 mm in
diameter. The question is how the pits are formed and
persist during the surface etching. It has been observed
that deep etching has the same effect at pores as at
inclusions (i.e., they are enlarged by a factor of 10). It is
therefore likely that a pit in itself enhances the chemical
reaction as in pitting corrosion (e.g., by increasing the
concentration of reactive ions). The start of this reaction
may differ depending on the type of inclusion. For
oxides, spinels, and boride clusters, pores often are
associated with the inclusions,[2,3,6] and these pores can
initiate the reaction. The alkali solution also lowers the
surface tension, helping the solution penetrate gaps or

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 42B, FEBRUARY 2011—127

Fig. 10—(a) Typical microscopic appearance of various inclusion types found in a 6063 billet. Micrographs showing the dominant inclusion
types in a billet: (b) TiB2 cluster in bottom disc; (c) agglomerated oxide films in top disc. (d) Optical images of inclusions and pores in the sam-
ple from the billet bottom.

cracks between inclusion and matrix. For carbide
inclusions, a reaction likely occurs between the OH ions
and the carbide to form methane,[23] thereby initiating
the pitting reaction.
Intermediate phases, such as AlFeSi and Al3Ti,
obviously do not react in the same way. Their corrosion
potential differs from that of the matrix and they react at
a different rate, probably because of good coherency
with the matrix; however, the solution does not pene-
trate any gaps and no pitting reactions start. Neverthe-
less, the method can be regarded as effective at detecting
inclusions.
This novel technique has obvious advantages over the
common microscopic analysis method in terms of easier
specimen preparation, larger areas analyzed, and fairly
quantitative results. Consequently, the total inclusion
distribution in an ingot can be determined relatively
quickly, facilitating efforts to improve inclusion control.
The method has some limitations; for example, it is so
far difficult to distinguish between inclusion types based
on etch pit shape. In addition, during deep etching,
porosity produces an effect similar to that of inclusions;
for porosity, however, the surface area of the pits
increases more with time than does the depth, resulting
in shallow pits. In addition, several even shallower pits
occur and are observed under optical microscopy, which
are likely associated with dislocations. These pits are not
visible to the naked eye and do not disturb the analysis.

128—VOLUME 42B, FEBRUARY 2011 METALLURGICAL AND MATERIALS TRANSACTIONS B

Fig. 11—Prefil flow curves and metallographic analysis results corresponding to tests 1 and 2.

Table I. Total Inclusions and Oxide Films Obtained from Residue of Prefil Sampling

Experiment Filtered *Total Inclusions Oxides *Harmful Inclusions, Volume Fraction,

Number Metal (kg) (mm2 kg–1) (# kg–1) Total Without Grain Refiner 9 10–6 Eq. [3]
1 1.08 0.741 32 0.156 18.5
2 1.4 0.234 11 0.023 5.8
3 1.4 0.627 33 0.107 15.6
*‘‘Total inclusions’’ include all types of inclusions existing in the ‘‘cake’’ above the filter, whereas ‘‘harmful inclusions’’ are the total number,
minus the number of inclusions associated with grain refinement (i.e., the sum of Al4C3 > 3 lm, dispersed Al2O3, MgO, and MgAl2O4).

which is in the range of harmful inclusions sizes,[4,9] to

be detected by the naked eye.
Finally, as the holes are easy to observe, one can
envisage various techniques to scan the etched surface to
detect the holes using an image analysis program. It also
may be possible to develop an automatic technique to
characterize the total inclusion distribution on a large-
sized sample.

2. Prefil footprinter method

Fig. 12—Optical micrograph showing TiB2 inclusions in the filter
from Prefil test 1.
In Figure 3, an etch pit corresponding to a TiB2
cluster was identified. From such images, one can
estimate a correlation between the microscopic and the
macroscopic scales (i.e., correlate the etch pit size with
the initial inclusion size). Deep etching for 15 minutes
enlarged the initial inclusion size by approximately ten
times. Thus, this etching technique can be regarded as
effective at allowing inclusions larger than 20 to 40 lm,
The Prefil technique has the advantages of lower
instrument cost as well as the ability to analyze a larger
range of inclusions than the LiMCA analyzer. The
technique is based on the PoDFA principle, with the
addition of a real-time curve. This weight vs time curve
provides quick information on the quality of the molten
metal. In addition, the metallographic analysis of the
Prefil filters permits identifying the type, total inclusion
contents, and oxide film levels. The limitation of the
Prefil technique is associated with the need for careful
sampling. Differences in melt temperatures, alloys type,
and Prefil crucible preheating can affect melt viscosity
and, consequently, the filtration rate data[15] Further-
more, in the Prefil testing, the molten metal is taken
from a flowing stream with a ladle and poured into the
crucible containing the filter. The melt handling involves

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 42B, FEBRUARY 2011—129

disrupting the oxide skin, which may follow the
melt partly into the filter and influence the results.[24]
Godelweki and Zindel[25] have questioned the reliability
of Prefil results, and Cao[19] discussed factors that may
induce uncertainty in the Prefil tests.
B. Analysis of the Results
1. Deep-etching results
Typical results of characterizing the inclusion amount
and distribution on etched slices cut at various locations
along the length of a DC-cast billet were presented in
Figures 4 and 5. These figures show that the inclusions
are found more frequently in certain locations (i.e., the
bottom and top portions of a billet). The melt quality in
these parts of the billet depends largely on the condi-
tions at the start and end of the casting process, and
these portions normally are cut away and rejected
during industrial production. The higher densities of pits
in the billet bottom (i.e., at the beginning of the casting)
are related to the disruption of the oxide skin by the
strong turbulence when pouring the liquid aluminum
into the mould.[5,6] The slight increase in the inclusion
content at the top of the billet can be explained by the
disturbance of the melt flow at the end of the casting
process as the melt level in the launder system starts to
decrease. These obtained results were confirmed from
the metallographic analysis, which clearly indicated a
considerable increase in oxide inclusions in samples
taken from these parts of the billets (Figures 10(b)–(d)).
When counting the pits in each of the three size
ranges, as shown in Figure 7, most etch pits in the
bottom of the billet were large in diameter (i.e., of class
C > 0.4 mm), whereas most inclusions in the billet
interior were of class A (i.e., 0.2 < A > 0.3 mm). The
largest pits in the billet bottom were identified using
optical microscopy and were found mainly to be oxide
films.
The radial distribution across a 228-mm-diameter
billet (Figure 8) clearly indicated that, at every billet
height, more inclusions were found near the central zone
of the billet cross section than at the MR or the S. This
inclusion location trend is also obvious in the images
of deep-etched longitudinal sections presented in
Figures 6(a) and (b). The central zone of a billet is
formed in the last stage of solidification, which implies
that the inclusions can be pushed toward the center by
the fluid flow and possibly by the solidification front
during solidification from the chill mold toward the
center of the billet. These results are consistent with the
flow pattern discussed in Du et al.[26] In Figure 8, one
also can note that the bottom disc displayed two
maxima at both the center and the surface. The higher
inclusion density of a circular distribution nearer the
surface in Figure 4 and in Figure 6(a) is probably a
result of the prevailing flow conditions just after mold
filling coupled with the rapid solidification at the bottom
block. The inclusions in this circular pattern have been
identified using optical and SEM/EDX analysis as
mainly consisting of TiB2 particles but also can consist
partly of AlPO4 (bone ash). TiB2 particles are associated
with the grain refinement procedure, and an excess of
130—VOLUME 42B, FEBRUARY 2011
grain refiners often are added at the beginning of the
casting, which can result in the observed increase in etch
pits in this region.
Bone ash is used traditionally in the launders in billet
production. Because of its dewetting behavior, it may
become entrained by the molten aluminum flow. AlPO4
particles are so small that they are difficult to detect
using optical or SEM microscopy, and they also dissolve
in water during preparation.
From the varying inclusion distribution patterns
observed here, in both the axial and radial directions,
it is clear that taking a small (2 to 3 cm2) metallographic
sample somewhere in a billet section will not give a good
representation of the inclusion content in a casting. This
fact underlines the potential of the newly developed
etching technique.
2. Prefil results
The Prefil curves in Figure 11 are of different slopes
corresponding to different melt qualities. The sample
associated with the low curve contained more inclusions,
which gradually clogged the filter and reduced the
filtration rate (i.e., increased the time for melt flow
through the filter). The microscopic analyses performed
on the residue on the filter of the Prefil instrument
(Table I) confirmed the shape of the flow rate curves
(i.e., the slope decreases as the number of inclusions
increases).
The Prefil results also indicate that the melt has a
higher inclusion content before degassing (sample 3)
than after degassing for sample 2 but not for sample 1,
as presented in Table I. The higher content of Al2O3
oxides concentrated on the Prefil filter in test 1 may be
because Prefil sampling (i.e., skimming, tool dipping,
and melt pouring) disturbs the protective oxide skin
during the Prefil trial rather than representing an actual
melt quality.[24] These results indicate an uncertainty
associated with the use of the Prefil technique.
3. Metallographic examination
The microscopic analysis of inclusions from both the
Prefil residue and the billet samples revealed the
presence of magnesium oxides and spinels, which was
expected, as the studied 6063 alloys typically have a Mg
content of 0.4 to 0.55 pct.[27] The MgAl2O4 spinels are
the most detrimental inclusions in aluminum because of
their large size and hardness. In addition to the
prevalent oxides, TiB2 and Al4C3 inclusions also were
observed. The carbides form when reducing the pot cells
in the aluminum smelting process. Al4C3 inclu-
sions <3 lm are not considered harmful.[24] TiB2
agglomerations were present in a significant quantity
and formed as a result of AlTi5B1 grain refiner additions
to the molten alloy. TiB2 inclusions are hard and have
adverse effects on extrusion and machining tools. In
contrast, TiAl3 is soluble under normal conditions and is
therefore not considered inclusion forming.[4]
The detected oxides and borides were rather small in
the studied alloys as the studied molten alloy was refined
using degassing equipment (SNIF). For melts cleaned
using the SNIF technique, it has been demonstrated[28]
that oxides larger than 50 lm and borides larger than
METALLURGICAL AND MATERIALS TRANSACTIONS B
20 lm are removed, whereas the smaller borides are
agglomerated.
4. Deep-etching test vs other methods
It would be useful to compare the inclusion density
measured using the deep-etching method with the
density measured using other common inclusion assess-
ment methods, such as Prefil, PoDFA, and LiMCA. To
make such a comparison, the number of etch pits is
recalculated and expressed in the following units: in
mm2 kg–1 (i.e., inclusion area per kilogram of etched
metal) for the Prefil and PoDFA techniques and in
N kg–1 (i.e., number of etched pits in thousands per unit
weight) for the LiMCA technique. The mass of the
etched material can be obtained from the alloy density
and etched volume. The area of an etch pit was
determined simply by measuring its average mean
diameter. Thus, both the total area fraction on an
etched billet surface that the etch pits occupy and the
number of pits per unit weight can be calculated easily
using the following equations:
A order of magnitude.
Area=Weight ðmm2 =KgÞ ¼ N 
m sions in liquid metals can be calculated from Prefil-
pR2p pR2p
¼N ¼N
q  Vm q  pR2  t
½1
N
Number/Weight ðN=KgÞ ¼ ½2
m Sv ¼ dqf X
where N is the number of etch pits, A is the surface area
of the pits (assumed to be of a circular cross-sectional
area in two dimensions), m is the mass of the etched
materials, q is the alloy density, V is the etched material
volume, Rp is the pit radius, R is the billet radius, and t is
the etched depth. Here, a layer of 0.3 mm is removed
after 15 minutes etching (i.e., t = 0.3 mm).
The inclusion levels measured in the melt using the
Prefil instrument were compared with the inclusion
measurements made using the deep-etching method.
Prefil data for test 1 corresponds to a 228-mm-diameter
billet slice taken 1.6 m from the bottom block and for
test 2, which corresponds to a slice taken at 4 m from
the deep-etched values in mm2 kg–1 (obtained using
Eq. [1]), at these billet positions were 73 and 75 mm2 kg–1
and correspond to the Prefil values of 0.741 and
0.234 mm2 kg–1, respectively. The calculated deep-
etched values per unit weight are much higher than
those of the Prefil samples, mainly because the etch pit
size and the initial inclusion size need to be correlated.
The etch pits are on average ten times larger than the
inclusion size measured microscopically, and the deep
etching also reveals inclusions in multilayers, giving
inclusion counts at least three times larger than those
determined by metallographic examination of a polished
surface. Taking these factors into consideration, the
calculated values of 73 to 75 mm2 kg–1 will be reduced
to approximately 2 mm2 kg–1. Therefore, the number of
inclusions determined by deep etching in the solidified
metal compared with the Prefil data are in the same
From Eq. [3],[29] the volume fraction of solid inclu-
Footprinter results. For a cylindrical filter medium with
a diameter (d) of 12.7 mm, a filtrate density (qf) of
2500 kg m–3, and an average inclusion density of
3500 kg m–3, the values obtained were given in Table I
and were calculated as follows:
p
½3
4
The etch pit counts also can be expressed in LiMCA units
N kg–1. At the same stages of casting the 228-mm-
diameter billet as previously described (i.e., at 1.6 and 4 m
billet lengths), the values obtained using Eq. [2] were 1030
to 1060 counts kg–1, respectively. These values agree
reasonably well with those found using industrial LiMCA
analysis, as is shown in Figure 13,[30] which range from
2000 to 6000 N kg–1 in an unfiltered melt. For the

Fig. 13—LiMCA data[30] compared with deep-etching data from Fig. 5. An average of 30 etch pits on a 152-mm-diameter slice from the bulk of
the billet (horizontal line) corresponds to an LiMCA value of 2100 counts kg–1.

METALLURGICAL AND MATERIALS TRANSACTIONS B VOLUME 42B, FEBRUARY 2011—131

152-mm-diameter billet, with an average of 30 etch pits
per slice for the main part of the billet (Figure 5), the data
correspond to an LiMCA value of 2100 N kg–1. In
Figure 13, the LiMCA data from Keegan et al.[30] also
are compared directly with the deep-etching data, as the
horizontal line corresponds to an average concentration
of 30 etch pits per slice from Figure 5.
V. CONCLUSIONS
A novel deep-etching method has been developed
and used to study nonmetallic inclusions in aluminum
DC-cast billets. This method of visually examining
whole billet cross sections displays good promise as a
new quality-control tool for cast houses, yielding rapid
analysis of the total inclusion content in solidified
products.
The technique reveals, in a relatively simple way and
with high accuracy, the variation in the content and
distribution of inclusions in aluminum billets in both the
lengthwise and the transverse directions. The results
indicate higher inclusion densities at the beginning and
end of billets. Radial inclusion distributions generally
indicate higher counts nearer the central axis of the
billets than at the midradius and the edge.
The obtained quantitative information on inclusion
locations can help aluminum cast houses to understand
the causes of impurity occurrence and to take preven-
tative measures to improve casting quality.
The novel deep-etching method produced more reli-
able data concerning the total inclusion content in billets
than did the Prefil method, and an attempt to compare
the method with LiMCA was reasonably successful.
Moreover, the new method also determines the distri-
bution of inclusions in the billets, not only the amount
as is the case with the other techniques.
ACKNOWLEDGMENTS
The Swedish KK Foundation and the European
Regional Development Fund supported this research
financially. The authors are grateful to Kubikenborg
Aluminium AB for providing the sample materials and
for stimulating discussions.
132—VOLUME 42B, FEBRUARY 2011
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