Quality-oriented

melt testing
in the
aluminium foundry

Certified
according to
DIN EN ISO 9001
DIN EN ISO 14001

Quality-oriented melt testing in the aluminium foundry15)

Mistakes in the melting process can seriously affect quality. Up to the present, it
was possible to monitor this process more or less successfully using the hydrogen
and dross tests only. With the vacuum density test, the foundryman now has a
much more reliable and convenient means of monitoring the quality of his melt.
This article describes how this process is used for melt testing during the melting
process itself, and during melt treatment and transport. In addition, it also describes
the use of the laboratory pressure filter for analysing the oxide content, another
factor which has an important effect on melt quality.

Sources of error
in melting aluminium alloys
In foundries, mistakes are frequently made in melting
aluminium alloys. Of these the most important are listed
below:
1. Excessively slow melting of ingot and return material
which causes the semi-solid state to be maintained
too long1). This pasty state should be avoided. The
existing oxides of aluminium and of the alloy elements
are prevented from separating effectively from the
molten material. Most of them therefore remain in
the melt and form mixed oxides. It also causes
segregation and unduly high melting loss. This pasty
phase lasts especially long in in furnaces which are
overfilled i.e. whose charge is too great for their
capacity. This is often the case with electric resistance
furnaces which use cheap off-peak electricity.
2. The continuous charging of cold ingots and return
material leads to local cooling of the melt, thus causing
intermetallic compounds to separate especially mixed
crystals of iron and mangananese1),2) thereby causing
hard inclusions such as the hexagonal AlFeMnSi
crystals (which have a hardness of between 800 and
1000 HV) shown in fig. 1
1. Besides, the oxide coverings
of the ingots and return material cannot be separated
cleanly from the melt. The absorption of hydrogen is
also very high.
3. Return material in small pieces or with a slate-like
structure oxidises very rapidly when it comes into
contact with the melting flame. This creates oxide
flakes (fig. 2a) 1). Oxides in this enclosed form are
extremely difficult to remove from the melt. It only
becomes possible to clean the melt when the oxide
skins (fig. 2a)1) have been broken up.

Fig. 1: Compact hexagonal AlFeMnSi phase in an aluminiumsilicon alloy

4. Furnaces which are not kept clean offer oxides the

ideal opportunity to crystallise. Fig. 2b shows
crystallised oxides surrounded by amorphous oxides3).
The crystals consist of corundum (Al2O3) periclase
(MgO), spinel (MgAl 2 O 4 ), oxide hydrate (OAlOH),
zirconium oxide (ZrO2) and quartz (SiO2).
5. Furnace refractory linings which are unsuitable for
aluminium melts react with the melt and the reaction
products contaminate the melt. The metal burns into
the lining. When selecting refractory material for the
furnace lining, the amphoteric behaviour of the
aluminium is of great importance4).
6. No turbulence should arise when aluminium melts are
being transferred or transported. The stream of metal
must be laminar and uninterrupted. Launders and pipe

Fig. 2a) Accumulation of oxide skins in die-casting structure; b) crystallised oxides surrounded by amorphous oxides; c) oxides and
bubbles in die-casting structure

systems should be used to prevent the melt from

falling freely. Turbulent metal flows entrap air as well
as the oxide layer of the metal itself which is constantly
being re-formed. Fig. 2c shows the oxide skins and
bubbles which can form in the structure of die
castings through incorrect transfer of metal from one
container to another5).
7. Temperatures of over 850 C cause considerable harm
to the aluminium melt. At high temperatures the
absorption of gas and oxides increases dramatically.
Melt quality can also be impaired by incorrect
modification and grain-refinement processes.
Testing the melt quality
The above errors substantially reduce the quality of the
melt. Up till now, this could only be verified by the
hydrogen and dross tests with a greater or lesser degree
of success. However, the vacuum density test is a simpler
and much more reliable means of monitoring the quality
of an aluminium melt.

Fig. 3: Filling the crucible in the vacuum chamber

Measurement of the melt quality using

the vacuum density test
In the vacuum density test, a quantity of approximately
80 g of molten metal is allowed to solidify in a coated
iron crucible in a vacuum chamber under about 80 mbars.
The amount of time required for the metal to solidify
depends on the alloy in question and is generally about
6 minutes. The solidified sample is then weighed to
determine its density. The density measurements are
reproducible and give a reliable indication of the quality
of the melt.
Testing at 80 mbars has proved to be ideal. At lower
pressures the samples react too sensitively and at higher
pressures too sluggishly.

Fig. 4: Density samples of a melt solidified at atmospheric

pressure and a pressure of 80 mbars

Procedure
The procedure used for the vacuum density test is as
follows:
- Remove the liquid metal (at least 120 K above liquidus
temperature) from the well-skimmed melt and pour it
into the previously coated iron crucible which has been
heated to a temperature of around 100C (fig. 3)
3);
- Close the vacuum chamber;
- Allow the melt to solidify at 80 mbars;
- When the sample has solidified, release the vacuum
and remove the lid of the chamber;
- Lift the crucible out with tongs and allow the sample
to cool for about 2 mins in the crucible;
- Remove the sample from the crucible;
- Quench the sample in water;
- Measure the density of the sample.
Calculation of density
The density of the sample is determined using the
principle of Archimedes. The sample is suspended freely
on a nylon thread above the water vessel on the weighing
machine. The weighing machine is tared with the water
vessel including contents. The weight of the sample
suspended in water (i.e. the volume of the sample) is
then measured. The sample is then lowered onto the
bottom of the water vessel and its weight measured.

The ratio of weight to volume yields the density of the

sample.
The influence of pressure on the structure of a sample
of G-AlSi7Mg with strontium modification is shown in
fig. 4
4. The sample solidified under atmospheric pressure
has a much denser structure and therefore a higher
density of 2.62 g/cm3. The sample solidified at 80 mbars
on the other hand has a looser more porous structure
and a lower density of 2.35 g/cm3. The 10 percent
difference in density of the two samples is too great to
be able to make a sound casting. It should be no greater
than 4%. Experience shows that a minimum density of
the sample solidified at 80 mbars has to be maintained.
Melts with lower densities do not yield good castings.
The minimum densities for the various casting alloys are
as follows:
- aluminium-silicon alloys
2.55 g/cm3
- aluminium-copper alloys
2.65 g/cm3
- aluminium-magnesium alloys
2.55 g/cm3
- aluminium-zinc-silicon alloys
2.75 g/cm3
- aluminium-zinc-copper alloys
2.65 g/cm3

Results of the vacuum density test

The following examples show how accurately the vacuum
density test reflects the quality of the melt.
Fig. 5a shows the relation between the density of
the samples of G-AlSi7Mg solidified under 80 mbars,
(unmodified and continuously strontium modified7)-9),
and the hydrogen content determined by hot extraction.
The values for the two melts lie on different straight lines.
Fig. 5a indicates the following: for a melt hydrogen
content of for example 0.16 ppm, the modified sample
has a lower density of 2.40 g/cm3 than that of the
unmodified sample at 2.52 g/cm3. Expressed differently:
for a specified density of 2.55 g/cm3 an unmodified melt
may have a higher hydrogen concentration (0.144 ppm)
than the modified melt (0.114 ppm).
Fig 5b shows the relation between the densities of
samples solidified at 80 mbars from the pore volumes
of the permanent-mould and sand-cast test bars of
various solidification times made from the alloy
G-AlSi7Mg continuously modified with strontium. As the
pore volumes in castings is strongly dependent on the
conditions of solidification such as local solidification
times and temperature gradients, each test bar has its
own curve. The solidification times of the test bars are
17, 88 and 92 secs. Fig. 5b indicates the following: for a
specified density of 2.55 g/cm3 , the pore volume of the
permanent mould test bar (17 s) is 0.10 %, that of the
permanent mould test bar (88 s) is 0.32 %, and that of
the sand-cast test bar (92 s) 0.72 %. A specified pore
volume is therefore achieved by more rapid solidi-fication
and lower densities. For a specified pore
volume of
0.30%, the 17-sec. bar requires a density of 2.37 g/cm3,
the 88-sec bar 2.55 g/cm3, and the 92-sec bar 2.63 g/
cm3.
Fig. 5c on the other hand shows how the melt
quality depends on the melt treatment and how it
can be monitored by means of the vacuum density test.
250 ppm of strontium metal are added are added to
a
melt of G-AlSi7Mg at 780 C and a density of 2.6 g/cm3.
The strontium burn-off was not recorded. This caused
the density to decline to approx. 2.35 g/cm3. The quality
of the melt improved by allowing it to rest. The density
values increase again and the required value of 2.55 g/
cm3 is again achieved.
Fig. 5d shows an example of how the vacuum
density test can be used to monitor the quality of a
cylinder-head alloy G-AlSi5Cu3Mg in the casting furnace
during chlorination and holding. Immediately after
transfer of the melt from the rotating to the casting
furnace, the melt has a density of 2.11 g/cm3. During
the adjustment of the chemical composition lasting 150
minutes, the density rose to 2.20 g/cm3. After 60 minutes
treatment with chlorine, the density increased further
to 2.48 g/cm3. A further holding phase caused it to
increase still further to 2.70 g/cm3.
The vacuum density sample shows how incorrect
transfer of the melt causes the quality to deteriorate.
The cylinder-head alloy G-AlSi5Cu3Mg (density 2.65 g/cm3)
was poured freely from a furnace into a ladle. The height
of the fall was 2.10 metres. Following such
a
turbulent transfer, the density of the melt in the
ladle
was only 2.43 g/cm3. When a specially designed system
of pipes was used to transfer the metal, the quality of
the melt in the ladle improved to a density level of 2.55
g/cm3.
4

Fig. 5. Relation between density and hydrogen content

(measured by hot extraction) of samples solidified at a pressure
of 80 mbars (a), between density and pore volume of permanentmould and sand-cast test bars (b); assessment of melt quality: c)
during the melt treatment; d) of a cylinder-head alloy during
adjustment of chemical composition, chlorine treatment and
holding

a)
b)
c)
Fig. 6. Three types of oxide: (a) compact oxide, (b) flaky oxide, (c), (d) oxide skin

d)

Laboratory pressure filter

The values of the vacuum density samples are
determined mainly by the hydrogen and oxide contents.
The oxides are divided into three types, compact oxides,
flaky oxides and oxide skins (fig. 6)
6). The first two types
are relatively easy to remove from melts. Oxide skins such
as fine oxides (otherwise known as plankton) on the
other hand are not. These can be removed satisfactorily
by means of chlorinating reduction-type fluxes which
release chlorine and carbon oxide in the melt10). A good
indicator of the type of oxides which contaminate the
melt is the laboratory pressure filter (fig. 7)
7).
By means of the laboratory pressure filter, the
inclusions in 4 kg of melt are concentrated on 1 cc of
filter residue. This is equivalent to a concentration factor
of 1500. 0.3 to 0.6 bars of pressure are applied with argon
to 6 kg of melt in an iron crucible. The base of the crucible
is fitted with a filter holder containing a ceramic filter of
Mullit-12011) with an average pore size of 15 m. The
metal forced through the filter is caught in a vessel which
is placed on an electronic weighing machine. When 4 kg
of melt have passed through, a solenoid valve is opened
automatically and the pressure declines. The solidified
melt residue and the ceramic filter are sawn apart (fig.
8)
8). The inclusions in the 10-mm thick metal residue on
the filter are released by the bromine-methanol process
and then identifed using a microprobe or other method
of analysis.

Fig. 7. Laboratory filter for enrichment of melt inclusions

Examination of the inclusions

Fig. 9 shows a pore in the strontium-modified alloy GAlSi9Mg12). Under strong magnification, a compact oxide
particle is visible to which the formation of the structure
pores can be attributed. The microprobe examination
reveals that the core is of aluminium oxide (Al 2 O3 )
surrounded by magnesium oxide (MgO). Enclosed in the
oxide are potassium, calcium and traces of phosphorus.
Titanium and boron (probably in the form of titanium
diboride from grain refining agents) form a layer around
the oxide.
In fig. 10
10, we see an oxide skin inclusion in strontiummodified G-AlSi9Mg as well as the results of the
microprobe analysis. The core consists for the most part
of aluminium oxide (Al2O3) and magnesium oxide (MgO)
in which strontium, sodium, potassium and calcium are
embedded. Titanium, boron and traces of carbon form
a coating surrounding the oxide. Titanium and boron are
present in the surrounding coating in the form of
titanium diboride. This in turn originates from the grain

Fig. 8. Cross section through ceramic filter with metal above.

It shows the concentration of inclusions at two different
magnifications

refining agent which in this form has no further grainrefining effect.

Fig. 11 shows a flaky inclusion in the secondary alloy
G-AlSi12(Cu). This a complex agglomerate of oxides,
phosphite, phosphate, silicate and titanate. It also
contains barium, sulphur, manganese and iron. Inclusions
of this type are formed on the walls and at the bottom
of furnaces and crucibles when these have not been
properly cleaned.
5

Fig. 9. Pore in structure of strontium-modified G-AlSi9Mg, composition photograph and x-ray distribution plates

Fig. 10. Oxide-skin inclusions in structure of strontium-modified G-AlSi9Mg, composition photograph and x-ray distribution plates

Fig. 11. Flaky inclusion in the secondary alloy G-AlSi12(Cu), composition photograph
and x-ray distribution plates

In fig. 12
12, a compact inclusion in the secondary alloy
G-AlSi12(Cu) is shown alongside the results of the
microprobe analysis. The hardness test produced results
of 550, 657 and 707 HV and the microprobe analysis
contents of Al2O3, SiO2, oxygen and potassium. It is a
potassium-aluminium silicate. This inclusion is also
formed on the walls and bottom of furnaces and
crucibles in the course of time.
6

The accumulation of oxide skins and impurities in the

secondary alloy G-AlSi12(Cu) in fig. 13 consists of
aluminium oxide, silicon oxide, magnesium oxide and
sodium. Spinel is also present.
The composition photograph (atomic composition of
the surface) and the x-ray plates showing the distribution
of various elements (fig. 14) reveal the soft inclusion in

Fig. 12. Compact inclusion in the secondary alloy G-AlSi12(Cu), composition photograph and x-ray distribution plates

Fig. 13. Accumulation of oxide skins and impurities in the secondary alloy G-AlSi12(Cu),
composition photograph and x-ray distribution plates

Fig. 14. composition photograph and x-ray distribution plates of a soft inclusion in a bright-polished cast surface.

a bright machined casting surface to be strontium oxide.

Besides the main constituents strontium and oxygen,
significant quantities of potassium and carbon were also
demonstrated. The carbon is present in the fragmentary
transverse folds of the inclusion and is obviously due to
coolants used during machining of the casting13),14).
Conclusion

three types of oxide: compact and flaky oxides as well as

by oxide skins. The structure and composition of these
oxides is also described.

Bibliography:
) H i e ls c h e r, U . : Aluminium 59, 1993, Nr. 7, 531-535.
) H i e l s c h e r, U . ; A r b e n z , H . ; D i e c k m a n n , H . :
Giesserei 53, 1966, Nr.5, S. 125-133.
3
) J o h n e , P.: Handbuch der Aluminiumzerspanung.
Dsseldorf 1984.
4
) R e g g , W.: Giesserei 49, 1962, Nr. 7, S. 157-162.
5
) H i e l s c h e r, U .: Schweiz. Alum. Rundsch. 1982, Nr. 5.
6
) H e c k l e r, M . : Aluminium 43, 1967, Nr. 4, S. 239-244.
7
) Alusuisse-Merkblatt: Code Ac-70/Ac-72/501.
8
) Alusuisse-Merkblatt: Code 601.
9
) Alusuisse-Katalog ber Httenaluminium-Gulegierungen.
Ausg. 1984.
10
) H i e l s c h e r, U . : Behandlung von Aluminiumschmelzen in
Gieereien und Httenwerken. Informationsschrift 27 der
Universitt-Gesamthochschule Duisburg. Moers 1982. S. 137-143.
11
) Filterkeramik-Merkblatt: Keramikfilter fr Trennprozesse.
12
) Alusuisse-Merkblatt: Code Sf-30/511.
13
) Alusuisse-Datenblatt: Spannungsrichtwerte fr das Drehen von
Gustcken aus Httenaluminium-Gulegierungen mit Hartmetall.
14
) Alusuisse-Datenblatt: Spanungsrichtwerte fr das Frsen von Gustcken aus Httenaluminium-Gulegierungen mit Hartmetall.
15
) H i e l s c h e r, U . : Giesserei Heft 23, 1987, S. 695-700.
1
2

This paper gives a brief review of the mistakes which can

be made during the melting process and their effects
on the quality of the melt. The monitoring of the melt
quality by means of the vacuum-density test is not only
more reliable but also less complicated. The paper
describes the application of the test process and the
monitoring of the melt quality during adjustment of the
chemical composition, chlorination, holding, transfer and
modification of aluminium-silicon alloys. The vacuum
density test allows reproducible measurement of the
effect of solidification times and temperature gradients
on the volume of pores in the structure of the casting
and of the hydrogen content on modified and
unmodified melts. The use of the laboratory pressure
filter for concentration of oxides in the melt is also
outlined. The quality of the melt is adversely affected by

grain size
degree of modification
solidification time

therma-analysis

inclusion
impurities
density index

vacuum density
ALSP III

TA 110

3 VT

weighing machine
MK 2200

computer communication with melt and production facilities

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