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Acta mater.

48 (2000) 2349±2362
www.elsevier.com/locate/actamat

A STUDY OF ALUMINIUM FOAM FORMATIONÐ


KINETICS AND MICROSTRUCTURE
I. DUARTE{ and J. BANHART{
Fraunhofer-Institute for Advanced Materials, Wiener Str. 12, 28359, Bremen, Germany

(Received 26 November 1999; accepted 20 December 1999)

AbstractÐAluminium foams were produced by applying the powder compact melting method, i.e. by mix-
ing metal powders and powdered gas-releasing blowing agents and pressing them to a foamable precursor
material after this. The resulting precursor was then foamed by heating it up to above its melting point
inside an ``expandometer'', which allowed for the volume and temperature to be measured throughout the
entire process. The present studies comprise the e€ects of the aluminium alloy composition (AlSi7 and
6061), some of the pressing parameters of the foamable precursor material, the foaming temperature and
the heating rate during foaming on the expansion behaviour of the foam. Moreover, the morphological
and microstructural evolution of metal foams is investigated. 7 2000 Acta Metallurgica Inc. Published by
Elsevier Science Ltd. All rights reserved.

ZusammenfassungÐAluminiumschaÈume wurden durch AufschaÈumen von Pulverpreûlingen hergestellt.


Dazu wurde eine Mischung bestehend aus Metallpulvern und einem gasabspaltenden Treibmittel in einem
ersten Schritt zu einem aufschaÈumbaren, dichten Vormaterial verpreût. Dieses Vormaterial wurde dann
durch ErwaÈrmung auf eine Temperatur oberhalb seines Schmelzpunktes aufgeschaÈumt. Das SchaÈumen
fand in einem ``Expandometer'' statt, das die Messung von Schaumvolumen und -temperatur waÈhrend des
ganzen Prozesses erlaubt. Untersucht wurde der Ein¯uû der Legierungszusammensetzung (AlSi7 oder
6061), einiger Preûparameter des Vormaterials, der SchaÈumtemperatur sowie der Heizrate auf das Expan-
sionsverhalten der SchaÈume. Auûerdem wird die Entwicklung der Porenstruktur des Schaumes und der
Mikrostruktur der ZellwaÈnde charakterisiert. 7 2000 Acta Metallurgica Inc. Published by Elsevier Science
Ltd. All rights reserved.

Keywords: Powder processing; Aluminum; Foams; Kinetics; Stability

1. INTRODUCTION product (called ``foamable precursor material'') by


hot pressing, extrusion, powder rolling or other
Cellular metals can be produced by a variety of
methods. In a ®nal step the foamable precursor ma-
di€erent methods [1]. Among these, metal foaming
terial is expanded by heating it up to above its melt-
methods are especially attractive because they allow
ing point. This transfers the metal into a semi-
for manufacturing fairly inexpensive closed-cell ma-
liquid viscous state and simultaneously makes the
terials with attractive mechanical properties. By blowing agent decompose, thus releasing gas and
``foaming'' one usually means releasing gas in a creating a highly porous structure.
liquid, ensuring that the gas bubbles do not escape Metal foams have been characterised thoroughly
and by ®nally stabilising the liquid foam by cooling with respect to their morphology, their mechanical
[2]. properties and to other properties important for po-
A manufacturing method for producing closed- tential applications [6, 7]. However, there is still
cell metal foams from metal powders was developed only very little work (see, e.g. Refs [8±10]) on how
some years ago [3±5]. The process consists of mix- the foam emerges from the liquid, how it changes
ing metal powder and a powdered blowing agent with time and what mechanisms are responsible for
and compacting the mix to a dense semi-®nished its formation. The present paper intends to help in
closing this gap.
Monitoring the foaming process of liquid metals
{ Now at Instituto Nacional de Engenharia e Tecnologia is much more dicult than doing the same with,
Industrial, Estrada do Pac° o de Lumiar, 1649-038, Lisboa, for example, aqueous foams. Many of the obser-
Portugal. vation techniques used for such foams cannot be
{ To whom all correspondence should be addressed. applied owing to the speci®c properties of liquid

1359-6454/00/$20.00 7 2000 Acta Metallurgica Inc. Published by Elsevier Science Ltd. All rights reserved.
PII: S 1 3 5 9 - 6 4 5 4 ( 0 0 ) 0 0 0 2 0 - 3
2350 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

Table 1. Some properties of the powders used. Dp means that p% of the particles are larger than the value given

Speci®cations by the powder supplier Measured powder properties

Powders Purity (%) Size (mm) D10 (mm) D50 (mm) D90 (mm) Mean diameter (mm) Oxygen content (%)

Al 99.7 < 160 128 57 17 67 0.7


Si n. spec. < 100 91 30 4.4 48 0.5
6061 alloy 99.5 60±400 250 116 59 140 1.1
TiH2 99 < 63 41 15 2.9 22 n. det.

metals: they are hot, opaque, very reactive with containing 0.6 wt% TiH2 (titanium hydride) were
oxygen and have a high electrical conductivity. This produced either by extrusion (for 6061) or by hot
rules out optical or resistometric methods which are pressing (for AlSi7). In both cases metal and blow-
often used for investigating aqueous foams [11, 12]. ing agent powders were mixed in appropriate quan-
One can distinguish two kinds of possible tech- tities in a tumbling mixer. Pre-alloyed air-atomised
niques for investigating the foaming process of 6061 powders (main alloying elements: 0.4±0.8% Si,
metals: ex situ measurements and in situ measure- 0.8±1.2% Mg, <0.7% Fe) were used for the ®rst
ments. In the ®rst case a foam is produced by heat- alloy, whereas AlSi7 alloys (which are similar to the
ing up a precursor thus initiating bubble growth casting alloys A356 or A444) were obtained by
and foam formation. After a given time the foam- blending elementary aluminium (also air-atomised)
ing process is interrupted by cooling and the result- and silicon powders. Table 1 lists some of the pow-
ing solid foam is characterised. By varying the time der properties. The ®rst two columns contain data
between the beginning of the experiment and the given by the powder manufacturer, whereas the
interruption of foaming, one obtains a series of powder size spectrum was measured with a Coulter
samples which re¯ect the various stages of foam particle size analyser, the oxide content with a Leco
evolution. The disadvantage of this approach is TC436 oxygen/nitrogen determinator by the
that it takes a long time to carry out such investi- authors.
gations and the results bear a certain inaccuracy For extrusion, 50 kg of the powder mix were ®rst
originating in statistical variations between the compacted to cylindrical slugs of 70±80% theoreti-
single experiments. Even if the starting materials for cal density by cold isostatic pressing (CIP) [13].
the individual foaming experiments were produced Although this step is not absolutely necessary, it
in the same way, each foaming experiment would helps to facilitate handling of the slugs and also in
turn out slightly di€erently due to e€ects such as avoiding de-mixing and contamination of the pow-
accidental agglomerates of the blowing agent, struc- ders. The slugs were then pre-heated to 3608C and
tural defects in the precursor material, impurities, extruded to rectangular bars of 160  20 mm2
etc. Therefore, in situ methods for characterising cross-section in a second step in which a horizontal
metal foams are preferred in which a parameter 25 MN direct extrusion machine was used. Tablets
characterising the foam is measured during the of 9 mm thickness and 31 mm diameter were
evolution of one single sample. Unfortunately, such machined out of the extruded bars for the foaming
measurements are very dicult to carry out and at tests.
the moment only the most simple parameter, the Hot pressing consisted of axially densifying the
foam volume, can be measured in situ. powder mixture in a cylindrical die in two steps (see
In the present work the evolution of foam
Table 2): ®rst the powders were ®lled into the die
volume, pore morphology (shape and size), and
and placed into a furnace which was pre-heated to
foam microstructure will be studied. Only the
the pressing temperature T. The mixture was then
volume is measured in situ, while pore morphologies
pressed at a constant pre-pressing pressure p1
and microstructures are characterised on samples
during which the temperature of the initially cold
that were quenched from di€erent evolution stages
powder and die rose to the furnace temperature T.
of a growing or collapsing foam.
After a given period t1 the pressure was increased
to p2 and the actual hot pressing took place for a
2. PREPARATION OF MATERIALS given time t2. The function of the pre-pressing step
Two aluminium alloys were used which have is to avoid the powders from uncontrolled oxi-
gained importance in metal foaming. The wrought
alloy 6061 is used whenever high strength and a Table 2. Hot pressing parameters for cylindical 32 mm die
good corrosion resistance are desired. The casting
alloy AlSi7 is applied in composite structures of Step Temperature Time Pressure
foam and aluminium sheets or tubes because it has
Pre-pressing 208C 4 T (variable) t1 (variable) p1=60 kN
a low melting point and a good foamability. Two Final pressing T (variable) t2 (variable) p2=90 kN
foamable aluminium alloysÐ6061 or AlSi7Ðeach
DUARTE and BANHART: ALUMINIUM FOAM FORMATION 2351

Fig. 1. Foamable 6061 (left) and AlSi7 (right) precursor material containing 0.6 wt% TiH2.

dation during heating to the hot pressing tempera- Alternatively, the cold furnace was ®rst closed
ture. The pressed samples were 10 mm thick and around the glass tube and after that the furnace
32 mm in diameter so that they could easily be was heated from room temperature to the desired
machined to the dimensions needed for the expand- temperature at a given rate. In this way tests at low
ometer …9  31 mm). heating rates could be performed.
Figure 1 shows optical images of the microstruc- For the foaming tests a piece of foamable precur-
ture of both foamable precursor materials after sor material was placed inside the steel mould and
pressing. One sees that the compacted powders are was then heated. The laser sensor that was attached
virtually pore free in both cases. Light grey TiH2 to the top of the quartz tube constantly measured
particles can be seen in the metal matrix of both the position of the upper side of the sample through
alloys. The darker angular shaped silicon particles the open top side of the mould, thus allowing the
are only observed in the metallic matrix of the rise of the emerging foam to be monitored. In ad-
AlSi7 alloy. Due to the diculty in distinguishing dition, the temperature of the expanding sample
TiH2 and silicon particles on optical micrographs, and the surroundings of the mould were constantly
EDX will be used in further work to help in identi- measured with thermocouples. Both the thermo-
fying these particles. couples and the laser sensor were connected to a
computer via an A/D interface. The data was
3. EXPERIMENTAL PROCEDURE recorded and analysed with a standard acquisition
programme which allows for a direct visualisation
The tests were performed by foaming the precur- of the data already produced during the experiment.
sor tablets inside a so-called ``laser expandometer'', The measurement of the volume V of the expanding
which is explained in Fig. 2. The metal foam is cre- melt together with the sample temperature Ts gener-
ated inside a small cylindrical steel mould (diam- ated a pair of functions V(t ) and Ts(t ) which
eter: 32 mm, height: 70 mm) which is open only at characterise the expansion kinetics. The measured
the top. The mould is located in the centre of a data can be displayed as a pair of functionsÐ[V(t ),
quartz glass tube (1400 mm long, 140 mm diameter) Ts(t )]Ðor as one function V(Ts) with the time as
where it is held by a sample support made of stain- an implicit parameter.
less steel. The heat source is a folding furnace with The calibration of the laser expandometer was
a cylindrical chamber of 140 mm diameter and carried out at room temperature using various
650 mm height. The furnace is guided by rails and samples of a known height. Empty runs without
can be slid around the foaming tube within a few any sampleÐi.e. measuring the distance between
seconds. For future applications the glass tube can laser sensor and sample supportÐwere then per-
be operated under variable pressures and atmos- formed with the furnace at various pre-set tempera-
pheres and is therefore connected to a pump and tures to obtain the expansion characteristics of the
gas source. However, in the present study all foam- empty instrument, originating mainly in the thermal
ing took place at normal atmosphere. expansion of the sample support and the quartz
Two foaming procedures were applied: in the ®rst tube. The data was parametrised and stored. The
mode the furnace was pre-heated to the desired actual measurements on aluminium foam samples
temperature without the foaming tube being in it. could then be corrected automatically for the
After this, the hot furnace was closed around the expansion of the instrument using this correction
glass tube of the expandometer causing an immedi- data.
ate rise in the temperature at the sample site. This The acquired data were smoothed in order to
created the fastest possible temperature rise. eliminate noise coming from the laser sensor.
2352 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

Fig. 2. Schematic drawing of the apparatus used for the foaming tests (not to scale).

This noise is caused by thermal ¯uctuations in 4. RESULTS AND DISCUSSION


the atmosphere inside the glass tube during
4.1. Reproducibility tests
foaming. Smoothing with a time constant in the
order of a few seconds removed much of this As foam growth is a statistical process, two
noise. Moreover, the laser expandometer some- foaming experiments will never yield exactly the
times showed strong ¯uctuations in the heating same result, even if the initial conditions were
phase before foaming and, occasionally, even ``identical'', i.e. the same within the limits of exper-
negative volume readings (see, e.g. Fig. 4). These imental accuracy. Accidental agglomerates of blow-
are not real expansion e€ects but artefacts hav- ing agent particles in the foamable precursor or
ing their origin in the strong turbulences in the unpredictable heat transfer between the heat source
furnace, which mainly occur when it is heated and the foamable precursor samples are possible
up from room temperature. In later stages of the sources for irreproducibilities. Moreover, the exper-
experiment the turbulences diminish because the imental set-up might contain elements which limit
temperature distribution in the furnace becomes reproducibility of foaming experiments, such as, e.g.
more uniform and stationary and therefore these friction e€ects between foam and mould which are
unwanted e€ects disappear. hardly reproducible. In order to get an idea of how
The laser sensor could measure distances with an reproducible foaming tests can be, four samples of
accuracy of 0.1% and a resolution of 0.02%. In the 6061 precursor material which were machined out
present application, however, this accuracy was not of the same extruded rod were foamed at the same
achieved because of the e€ects already mentioned nominal furnace temperature. Figure 3 shows the
and is not even necessary because of the nature of resulting temperature and volume curves for these
the foam surface which is uneven, curved and con- samples as a function of time. What is obvious is
stantly changing due to expanding and coalescing that there is a scatter on the time scale of the di€er-
bubbles. Therefore, no meaningful interpretation of ent expansion curves. One reason for this is that the
e€ects on a length scale of less than about 1 mm data recording programme was started only after a
can be given. certain delay time, after the furnace had been closed
DUARTE and BANHART: ALUMINIUM FOAM FORMATION 2353

We conclude that foaming tests can be carried


out in a reproducible way. However, di€erences in
maximum foaming height of less than 5 mm seem
to be insigni®cant. In practical tests we always car-
ried out a minimum of two tests on identical
samples and compared the results. If there seemed
to be too much di€erence between the two results,
(e.g. signi®cantly more than the di€erence between
the samples in Fig. 3), further tests were carried
out. However, if the curves were similar in this
sense an average curve was calculated. All volume
expansion curves shown in the next sections are
averages of at least two individual measurements.
Fig. 3. Reproducibility tests on four 6061 samples foamed
at 8008C. Left: time-resolved expansion and temperature,
right: expansion vs temperature.
4.2. Comparison with previous results
around the foaming tube, to allow the vibrations In previous studies the foaming process of alu-
caused by the furnace movement to be damped out. minium alloys was characterised by means of an ap-
Therefore, the sample temperature at t ˆ 0 is higher paratus which used a ceramic movable piston
than room temperature in all cases. This in¯uence instead of a laser [14, 15]. The expanding foam dis-
together with the possibly di€erent heat transfer placed the piston and generated the volume expan-
rate between mould and sampleÐwhich depends on sion function V(t ) this way. The aim of the ®rst test
whether the sample touches the mould only at some was to compare expansion curves given by this
points or with signi®cant parts of its surfaceÐ (old) expandometerÐcalled the ``mechanical
causes the observed shift of the various V(t ) curves expandometer'' and the one using the laser sen-
against each other. Maximum expansion occurs sorÐcalled the ``laser expandometer''. For this, var-
between 620 and 700 s after the start of data acqui- ious foamable precursor samples, as described in
sition. Nevertheless, all samples show almost the Section 2, were used [10].
same maximum expansion of about 50 mm. If one The results can be summarised as follows:
eliminates the time by plotting V(T ) (see right hand both data sets show the same stages of foam
side of Fig. 3) the foaming behaviour of all alloys formation, namely: (a) below the solidus tempera-
appears almost identical. ture of the aluminium alloy the expansion is

Fig. 4. Expansion curves of AlSi7 samples prepared at di€erent hot pressing temperatures. Other par-
ameters as given in Table 2. Absolute and relative densities of the hot pressed precursor samples are
given (theoretical density of fully dense alloy=2.68 g/cm3).
2354 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

small; (b) as the solidus temperature of the alu- compaction parameters on the kinetics of the foam-
minium alloy is reached, it starts to soften and ing process, samples of foamable precursor material
expands slowly as a consequence of the de- were prepared under di€erent conditions and
composition of TiH2 to H2 gas and Ti; (c) as the characterised in the laser expandometer. As the con-
temperature increases, the expansion rate increases ditions in the extrusion process could not be varied
rapidly until the maximum expansion is reached; easily because a full-size industrial extrusion ma-
(d) ®nally, the blowing agent is exhausted and no chine was used and batches of usually more than
longer releases hydrogen and the foam starts to col- 100 kg have to be produced each time, the par-
lapse. However, there are also some di€erences ameter study was carried out only with hot press-
between the curves obtained by the two instru- ing, which allows for the production of small
ments, namely: (a) the mechanical expandometer batches and therefore a larger number of di€erent
shows a lower maximum expansion due to the parameters can be varied. Foamable AlSi7 precur-
weight of the piston (9 g) and e€ects counteracting sor tablets of the required size were pressed, as
expansion, originating in friction between the pis- described in Section 2, for various pressing par-
ton, the emerging foam and the con®ning steel ameters (see also Table 2). After pressing, foaming
tube. Moreover, the laser measures the position of tests were carried out using a pre-heated furnace at
the centre of the expanding foam. As the foam 7508C.
expands without any restriction in the vertical direc- Figure 4 shows expansion curves of samples
tion, the surface of the foam is usually vaulted and which were pressed at di€erent hot pressing tem-
the highest point of the foam generates the distance peratures T, ranging from 200 to 5508C, with con-
reading. Values given by the laser expandometer stant pressing times t1 and t2. Figure 5 shows
therefore tend to be slightly too high (approxi- expansion curves of samples which were hot pressed
mately 2 mm); (b) in the collapse regime the mech- at di€erent pre-pressing and hot pressing times t1
anical expandometer yields constant volume and t2, but at a constant hot pressing temperature
readings because the piston is blocked soon after of 4508C. The pressures p1 and p2 were kept con-
collapse has begun. stant in all the tests.
From the comparison of the two instruments one It is obvious that the hot pressing temperature is
can conclude that the laser sensor is a more sensi- a critical parameter for the foaming behaviour
tive tool to measure the expansion during the entire (Fig. 4). The highest expansions are reached for hot
foaming process than the mechanical expandometer, pressing temperatures between 400 and 4508C. For
because it does not disturb the foam during its higher and lower temperatures the maximum expan-
growth and collapse. sion is lower and in the extreme case, for 200 and
5508C, virtually no foaming can be observed any
4.3. In¯uence of compaction conditions more. The reason for this is that for low compac-
tion temperatures only insucient densi®cation
In order to evaluate the e€ect of some of the with a high degree of residual open porosity is

Fig. 5. Expansion curves of AlSi7 samples prepared with di€erent pre-heating (t1) and hot pressing
times (t2). The hot pressing temperature was 4508C in all cases.
DUARTE and BANHART: ALUMINIUM FOAM FORMATION 2355

achieved, corresponding to a low density of the foaming tests were performed using a pre-heated
foamable precursor material (see values given below furnace which was slid around the glass tube con-
Fig. 4). Thus hydrogen gas can escape from the taining the sample for the test. The nominal furnace
melting precursor through the system of intercon- temperature was varied between 600 and 8008C.
nected channels and it does not create and in¯ate Figure 6 shows the in¯uence of temperature on the
bubbles. About 1% residual porosity appears to be foaming behaviour of the two aluminium alloys stu-
the tolerable limit for this particular alloy system. died. The curves are labelled with the nominal fur-
At the other extreme, too high compaction tem- nace temperature which, however, does not coincide
peratures also lead to lower maximum expansions with the sample temperature at any time. Heat
because hydrogen is lost already during hot com- losses through the ends of the cylindrical furnace,
paction. This loss is almost complete for a compac- which are closed by the glass tube, are the reason
tion temperature of 5508C. Thermoanalysis of free that even after a long test time the sample tempera-
TiH2 powder shows that decomposition begins at ture is lower than the nominal furnace temperature
3808C and continues up to 5708C. However, these by 35±508C. In further discussions we shall there-
results are valid only for free powders and depend fore also refer to the ®nal temperature in the
also on the heating rates applied in the tests and on sample. In Fig. 6 the solidus and liquidus tempera-
the environmental atmosphere. The optimum hot tures of the two alloys are shown as horizontal
pressing temperature, around 400±4508C, is there- dotted lines. The values measured by calorimetry
fore near the initial decomposition temperature of (AlSi7: 577/6208C; 6061: 610/6648C) deviate slightly
free TiH2 powder, but this does not harm the TiH2 from what one expects from the literature [16, 17]Ð
embedded in the gas-tight embodiment of the met- in particular the measured liquidus temperature is
allic matrix of the foamable precursor material. about 108C too highÐbut this does not change the
It is interesting to note that the samples com- conclusions.
pacted at temperatures TR4508C show a transient It is evident that the foaming process is sensitive
expansion peak after which the foam quickly to the foaming temperature chosen. If the ®nal
relaxes by a few millimetres to reach an almost con- sample temperature is below the solidus tempera-
stant volume (marked in Fig. 4). This peak could ture of the alloy (T1 for AlSi7, T2 for 6061) there is
be a consequence of excess hydrogen in the precur- not very much more of an e€ect than a slight solid
sor material which is weakly bound and is released state expansion. If the ®nal temperature lies in the
at an early stage of foaming. The excess hydrogen solidus/liquidus interval (T2 for AlSi7, T4 for 6061)
could possibly cause a too quick in¯ation of pores foam formation can be observed, but especially for
and a corresponding partial collapse of some thin- 6061 it is limited to quite low expansions around
walled membranes. The sample pressed at 5008C 100%. The viscosity of the semi-molten material is
does not show this behaviour and reaches a stable still quite high at this temperature and surface oxi-
state without showing the transient peak. This is dation leads to an additional resistance towards
understandable since compaction of the powder mix bubble in¯ation, counteracting the internal gas
at 5008C is just sucient to drive out this excess pressure built up by the decomposing blowing
hydrogen, while this temperature is still too low to agent. Increasingly higher temperatures reduce vis-
remove all the blowing gas. This, however, happens cosity and promote gas production so that higher
at 5508C compaction temperature. From the and higher volume expansions can be observed.
measurements one can therefore conclude that the Beside reducing viscosity, high furnace temperatures
blowing agent content of 0.6 wt%Ðusually used in naturally also lead to high heating rates. This can
the industrial production of foamable precursor ma- be advantageous for obtaining high volume expan-
terialÐis unnecessarily high and should be slightly sions as will be shown in the following section. The
reduced. As titanium hydride is quite expensive, this volume expansion seems to almost saturate out for
would help to reduce costs. AlSi7 at 7508C, whereas the maximum of foam
Figure 5 demonstrates that the compaction time expansion for the 6061 alloy is presumably at tem-
is a fairly uncritical parameter for the hot pressing peratures above the maximum temperature at which
temperature and pressure chosen. The expansion the furnace can be operated (8008C), as can be seen
curves are all quite similar, the remaining di€er- from Fig. 7 which displays the maximum expansion
ences being within the range of normal statistical as a function of nominal furnace temperature
¯uctuations. Tfurnace, ®nal temperature in the sample T®nal and
the temperature at the moment of maximum expan-
sion Tmax. exp.. The di€erence between nominal fur-
4.4. In¯uence of foaming conditions nace temperature and the ®nal sample temperature
has already been explained. Comparing the two
4.4.1. Furnace temperature. Foamable precursor temperatures T®nal and Tmax. exp. one can see that
samples of AlSi7 and 6061 alloys, as described in they are almost identical for low furnace tempera-
Section 2, were used for studying the in¯uence of tures, i.e. the temperature does not rise any more
the furnace temperature on foaming kinetics. The after the maximum of expansion has been reached,
2356 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

whereas for high furnace temperatures the sample 4.4.2. In¯uence of heating rate. Di€erent furnace
temperature continues to increase after maximum temperatures lead to di€erent heating rates and in-
expansion and therefore Tfinal > Tmax: exp : The latter ¯uence the foaming process this way. In order to
situation seems to be a prerequisite for obtaining evaluate the in¯uence of the heating rate indepen-
high expansion rates: one has to ensure a high heat dently of temperature, foaming tests were carried
¯ux into the sample up to maximum expansion by out at 8008C at di€erent heating rates. For this the
providing a furnace at a suciently high tempera- cold furnace was put around the glass tube contain-
ture. ing the samples before it was heated up at the given
The curves for AlSi7 in Fig. 6 show the same in- rate. Figure 8 shows three expansion curves
itial foaming peak which was already explained in obtained this way. The fourth curve corresponds to
the previous section. It only occurs for the higher the highest heating rate, which was obtained by
furnace temperatures. If the furnace is operated at using a pre-heated furnace at 8008C as described in
or below 7008C nominal temperature the excess the previous sections.
hydrogen can escape without creating an additional Clearly, higher heating rates lead to an earlier
expansion e€ect during the comparatively slow expansion of the foamable precursor material
heating phase. because the melting temperature is reached at an

Fig. 6. Expansion (E ) and temperature (T ) curves of AlSi7 and 6061 alloys foamed at di€erent nominal
furnace temperatures (600±8008C, values given in the legend). Solidus and liquidus temperatures of the
two alloys are given as horizontal dotted lines.
DUARTE and BANHART: ALUMINIUM FOAM FORMATION 2357

phology of 6061 and AlSi7 aluminium alloys during


foaming, a series of tests was performed in a pre-
heated furnace at 800 and 7508C, respectively.
These temperatures were derived from Fig. 6 and
ensure a good foamability of the two alloys. For
each sample of the series the foaming process was
stopped at a di€erent stage of evolution by remov-
ing the furnace from the quartz tube at a given
time, derived from the known volume expansion
curves for the respective alloys (given in principle in
Fig. 6, but re-measured for this purpose). After this
the metal foam specimens were quickly cooled to
room temperature. The expansion curve V(t ) and
the temperature T(t ) were recorded throughout the
experiment.
Fig. 7. Maximum foam expansions of AlSi7 and 6061
alloys given as a function of various temperatures Figures 9(a) and 10(a) show typical expansion
(Tfurnace=nominal furnace temperature, T®nal=®nal curves for the two alloys. The points marked with
temperature in the samples after 50 min of foaming, capital letters A±K and A'±K ' indicate the di€erent
Tmax. exp.=temperature in the sample in the moment of foaming stages that were prepared [to be more pre-
maximum expansion). cise, the stages at which the furnace was removed
from the glass tube. As there is a certain after-
earlier time. Beside this rather obvious di€erence expansion the samples were in a slightly more
the three expansion curves for the highest heating expanded state after cooling to room temperature
rates are very similar. Only a signi®cantly lower than indicated in Figs 9(a) and 10(a)]. In Figs 9(b)
heating rate leads to a change in the expansion and 10(b) the corresponding micrographs of the
characteristics, namely a lower maximum expan- various foaming stages are shown (the foamable
sion. The main possible reasons for the drop in precursor material is identi®ed by ``P''). As can be
foamability for low heating rates are: (i) gas losses seen from the micrographs, both aluminium alloys
due to the decomposition of titanium hydride show the same foaming stages, namely: (a) in-
during the slow transition through the temperature itiation and evolution of porosity: pores elongated
range from above 5008C, where decomposition is perpendicular to the compaction direction (which
rapid (see Section 4.3) and the temperature at was from top to bottom) are formed (phases A and
which foaming begins; (ii) oxidation which could A '); (b) pore growth: the pores are in¯ated by the
produce non-metallic layers on the surface of the evolving hydrogen and are increasingly rounded o€
precursor sample and even inside the sample in as the foam expands (B±G and B '±G '). The initial
regions accessible to air by direct channels. Such anisotropy starts to vanish until only a slight
oxide layers could contain alumina, magnesia or asphericity remains. Moreover, initially round pores
mixed oxides (6061 alloys contain magnesium), are deformed to more polyhedral pores as the level
which remain solid throughout the foaming process of porosity increases and no more space can be
and therefore mechanically hinder expansion. ®lled by spherical pores; (c) collapse: after maxi-
mum expansion no more hydrogen gas is released
and the foam begins to decay. This decay leads to
4.5. Evolution of pore morphology during foaming
foams with large and irregular pores, collapsed and
In order to observe the evolution of pore mor- oxidised pores especially at the top of the sample
and a solid metal layer at the bottom (see H±K and
H '±K ').
It is obvious that foam growth is neither isotropic
nor uniform in both alloys investigated. The aniso-
tropy has its origin in the texture created in the
powder compact during solidi®cation. In hot
pressed tablets always oblate pores are formed and
the following rise of the foam is along the original
axis of pressing, whereas round extruded rods (not
used in the present study) would rather expand in a
radial direction. Non-uniformities in the emerging
foam are probably caused by local agglomerates of
the blowing agent or structural defects in the pre-
cursor material created by insucient densi®cation,
Fig. 8. Foam expansion curves of 6061 alloys for di€erent impurities, or local oxidation. As the decomposition
heating rates at 8008C nominal furnace temperature. of TiH2 starts rather early at about 3808C, i.e. in
2358 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

the solid state, tiny voids in the precursor material ture is the reason for such processes but no de®nite
are formed, preferably near such structural defects, investigations have been carried out yet. It seems
and lead to the formation of heterogeneous pore that metal membranes are not as stretchable as,
morphologies in the subsequent foam expansion. e.g., the membranes in soap foams and rupture as
The foams owe their collapse to two mechanisms, soon as their thickness has fallen below a certain
drainage and coalescence. Drainage is the ¯ow of critical limit.
molten metal from the cell walls into the cell edges The collapse behaviour of the two aluminium
(driven by surface tension) and through cell edges alloys is quite di€erent. After maximum expansion
downwards driven by gravity [see H±K in Fig. 9(b) the AlSi7 foam does not loose its shape so much as
and H '±K ' in Fig. 10(b)]. A thick layer of metal at the 6061 foam. In the 6061 foam a thick layer of
the bottom of the samples is the result of this pro- metal at the bottom is formed. Moreover, the upper
cess. Coalescence occurs whenever two cells merge surfaces of the 6061 samples show more decay and
to form one large one. It is thought that cell rup- the vaulted shape disappears. In contrast, the AlSi7

Fig. 9. Expansion curve (a) and morphology at di€erent foaming stages (b) for 6061 alloys using a pre-
heated furnace at 8008C.
DUARTE and BANHART: ALUMINIUM FOAM FORMATION 2359

foam samples remain vaulted and maintain a more visible microstructural changes were expected in this
regular cellular structure throughout the entire test. material, initially containing two di€erent elemen-
tary powders. One question to be answered is how
alloying of the elementary particles takes place and
4.6. Evolution of microstructure during foaming
whether it is acceptable to use elementary powder
The microstructural evolution of the cell walls of mixes instead of the more expensive pre-alloyed
AlSi7 foam during the foaming process was investi- powders to make a given alloy foam. First of all
gated by analysing the samples described in the pre- the precursor material is revisited in Fig. 11. SEM
vious section. AlSi7 was chosen because more easily micrographs and an EDX-distribution map of sili-

Fig. 10. Expansion curve (a) and morphology in di€erent foaming stages (b) for AlSi7 alloys using a
pre-heated furnace at 7508C.
2360 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

Fig. 11. Large picture: SEM image of foamable AlSi7 precursor material (0.6 wt% TiH2). Aluminium
matrix (dark grey), silicon particles (light grey) and TiH2 particles (white) can be seen. The white frame
marks the area for which EDX element distribution maps are shown for Si and Ti (small pictures).

con and titanium were obtained. The SEM picture con distribution map (right column) shows that sili-
shows that although silicon particles of many di€er- con is spreading and forms increasingly larger Al±
ent sizes are present the distribution is quite uni- Si regions. This tendency continues for the further
form. The EDX element maps for silicon con®rms stages of foaming. After 50 min both the micro-
this observation. Moreover, it is important that the graph and the silicon distribution map show the
titanium (hydride) is also distributed quite uni- typical microstructure of a cast Al±Si alloy with
formly. light a-Al grains and heterogeneous Al±Si regions
Figure 12 shows the pore morphology, the micro- with their characteristic dark silicon needles [16].
structure and the silicon distribution at di€erent
foaming stages. The stages are marked according to
Fig. 10(a). Foaming times and sample temperatures 5. SUMMARY
are given in the column at the right.
Foaming stage A ' still shows individual angular The foaming kinetics of aluminium alloy foams
silicon particles (middle column, dark grey) produced by applying the powder compact melting
embedded in the aluminium matrix (white). Some route are determined by a complex interplay of sev-
pores (dark) can already be seen at this stage. As eral mechanisms which occur during the process.
the temperature is slightly below the eutectic line Foaming is strongly governed by temperature
(5778C) this is understandable. No liquid phase is e€ects: the expansion curve depends on the hot
present and interdi€usion times are long. Just 77 s pressing temperature for obtaining the foamable
later in phase B' the situation has completely chan- precursor material and the heating parameters
ged. The temperature is now 168C above the eutec- during foaming. Hot pressing the powders at 400±
tic temperature and the metals have formed an 4508C and using a furnace pre-heated to tempera-
alloy. The microstructure shows the typical a-Al tures well above the liquidus temperatures of the
grains (white) surrounded by a dark silicon-rich alloys investigated was found to yield the best
phase. Many of the grain boundaries are probably results. Making alloy foams from elementary pow-
identical to former powder particles as can be seen ders is unproblematic, at least for Al±Si alloys,
from the grain near the cell wall marked with `X'. because alloying of the elements takes place quickly
Although the powders are densi®ed during hot during foaming and a homogeneous microstructure
pressing, the oxide layers covering each individual is obtained after a short time. This is an important
powder particle survive even in the semi-liquid conclusion from the viewpoint of cost eciency.
state. The silicon-rich melt accumulates preferably
near such oxides, thus forming the observed grain
AcknowledgementsÐThe work was supported by the
boundaries. Another 77 s later in phase D ' we see a European Union (Marie Curie Training Programme ERB-
largely expanded foam at 6348C. The grains have BRMA-CT98-5103) and Deutsche Forschungsgemein-
grown slightly as compared to phase B' and the sili- schaft (Programme SPP-1075, Grant No. Ba 1170/3-1).
DUARTE and BANHART: ALUMINIUM FOAM FORMATION 2361

Fig. 12. Morphology (left column), optical micrographs (middle) and EDX silicon distribution (right
column) of AlSi7 foams at di€erent stages of expansion (not the same region of the sample shown in
di€erent columns). Letters denote the stage of expansion in which the furnace was removed from the
expandometer tube according to Fig. 10(a), the times and temperatures refer to that particular moment.
Note that due to the after-expansion after this the foams shown in the photographs are more expanded
than one would expect from the locations indicated in Fig. 10(a). Times are given in hh:mm:ss.
2362 DUARTE and BANHART: ALUMINIUM FOAM FORMATION

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