139
 Open Access. © 2019 Vončina M., Cvahte P., Kračun A., Balaško T., Medved J., published by Sciendo.  This work is licensed 
under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License. 
Received: Dec 03, 2019 
Accepted: Dec 16, 2019 
 DOI: 10.2478/rmzmag-2019-0018 
Original scientific paper 
Abstract
The alloys from Al–Mg–Si system provide an excellent 
combination of mechanical properties, heat treatment 
at extrusion temperature, good weldability, good cor-
rosion resistance and formability. Owing to the high 
casting speed of rods or slabs, the solidification is rath-
er non-equilibrium, resulting in defects in the materi-
al, such as crystalline segregations, the formation of 
low-melting eutectics, the unfavourable shape of inter-
metallic phases and the non-homogeneously distribut-
ed alloying elements in the cross-section of the rods or 
slabs and in the entire microstructure. The inhomoge-
neity of the chemical composition and the solid solu-
tion negatively affects the strength, the formability in 
the warm and the corrosion resistance, and can lead to 
the formation of undesired phases due to segregation 
in the material. In this experimental investigation, the 
cross-sections of the rods from two different alloys of 
the 6xxx group were investigated. From the cross-sec-
tions of the rods, samples for differential scanning cal-
orimetry (DSC) at three different positions (edge, D/4 
and middle) were taken to determine the influence of 
inhomogeneity on the course of DSC curve. Metallo-
graphic sample preparation was used for microstruc-
ture analysis, whereas the actual chemical composition 
was analysed using a scanning electron microscope 
(SEM) and an energy dispersion spectrometer (EDS).
Key words: casted rods for extrusion, homogeneity of 
chemical composition, DSC analysis, microstructure.
Analysis of Chemical Composition Homogeneity 
in the Cross-section of the Rods Produced from Alloys 
of 6xxx Group
Analiza homogenosti kemijske sestave po preseku litih drogov 
izdelanih iz zlitin iz skupine 6xxx
Maja Vončina
1,
*, Peter Cvahte
2
, Ana Kračun
2
, Tilen Balaško
1
, Jožef Medved
1
1
  Faculty of Natural Sciences and Engineering, Department for Materials and Metallurgy, University of Ljubljana,  
Ljubljana, Slovenia
2 
Impol Group, Partizanska 38, 2310 Slovenska Bistrica, Slovenia
* maja.voncina@omm.ntf.uni-lj.si
Povzetek
Zlitine iz sistema Al-Mg-Si zagotavljajo odlično kom-
binacijo mehanskih lastnosti, toplotno obdelavo pri 
temperaturi ekstruzije, dobro varivost, dobro koro-
zijsko odpornost in preoblikovalnost. Zaradi visoke 
hitrosti ulivanja drogov ali bram je strjevanje dokaj 
neenakomerno, kar ima za posledico nastanek napak 
v materialu, kot so kristalne segregacije, tvorba niz-
kotaljivih evtektikov, neugodna oblika intermetalnih 
faz in nehomogena porazdelitev legirnih elementov po 
preseku drogov ali bram in v celotni mikrostrukturi. 
Nehomogenost kemične sestave in trdne raztopine 
negativno vpliva na trdnost, preoblikovalnost v toplem 
ter korozijsko odpornost, poleg tega pa lahko vodi do 
tvorbe nezaželenih faz zaradi segregacije v materialu. 
V tej eksperimentalni preiskavi smo preučili prese-
ka drogov dveh različnih zlitin iz skupine 6xxx. Vzorci 
za diferencialno vrstično kalorimetrijo (DSC) so bili 
odvzeti iz prečnega prereza droga na treh različnih 
mestih (rob, D/4 in sredina), z namenom ugotavljanja 
vpliva nehomogenosti na potek DSC krivulje. Za anali-
zo mikrostrukture smo uporabili metalografski vzorec, 
medtem ko smo dejansko kemijsko sestavo analizirali z 
energijsko disperzijskim spektrometrom (EDS) na vr-
stičnem elektronskem mikroskopu (SEM).
Ključne besede: liti drogovi za ekstrudiranje, homoge-
nost kemične sestave, DSC analiza, mikrostruktura.

Vončina M., Cvahte P ., Kračun A., Balaško T., Medved J. RMZ – M&G | 2019 | Vol. 66 | pp. 139–148
140
Introduction
Aluminium alloys from the group 6xxx have 
good mechanical properties, good formability 
and corrosion resistance. Alloyed elements af-
fect weldability, corrosion resistance, corrosion 
cracking, electrical conductivity and density. 
Alloying magnesium and silicon to aluminium 
alloys from the group 6xxx takes place in the 
appropriate ratio (Mg/Si = 1.73) to form the 
Mg
2
Si phase [1]. In practice, alloys of the 6xxx 
system produced by casting techniques con-
taining excess silicon or magnesium. Excess 
silicon results in higher strength and increases 
their transformability but reduces corrosion 
resistance. Excess magnesium increases cor-
rosion resistance but reduces transformability 
and strength [2, 3].
The presence of iron in alloys of the 6xxx sys-
tem results in the formation of phases such as 
Al
3
Fe, Al
8
Fe
2
Si, Al
8
FeMg
3
Si
6
 and Al
6
Fe, which 
may be detrimental to the properties of these 
alloys [4]. Iron reduces ductility and toughness 
by forming coarse components with alumini-
um and other alloying elements. It also reduces 
strength, corrosion resistance and fatigue resis-
tance. The alloying elements of chromium and 
manganese correct the shape and size of iron 
phases and its compounds in alloys of the 6xxx 
system. The presence of manganese not only 
increases the temperature of recrystallisation 
and corrosion resistance but also allows dis-
persion hardening and ageing [2].
Although alloys from the group 6xxx have low-
er strength than alloys from the groups 2xxx 
and 7xxx, they have advantages such as good 
formability and corrosion resistance. Bismuth 
and lead can also be added for better machin-
ing by cutting. These alloys are used for profiles 
for doors, windows, ladders, walls and fences. 
They are used for the manufacture of frames for 
motors and cabinets of electric motors, heating 
and cooling pipes, office equipment, etc. [5].
The production of products from the alloys of 
the group 6xxx begins with the continuous or 
semi-continuous casting of the rods, followed 
by homogenisation. With a higher degree of 
homogenisation, better formability properties 
can be expected, which are crucial for further 
processing. Homogenisation annealing is the 
process by which crystal segregations and 
low-melting eutectics are eliminated, the shape 
of intermetallic phases is changed and small 
precipitates are formed. The homogenisation 
process achieves a uniform distribution of the 
alloying elements throughout the entire micro-
structure. The inhomogeneity of the solid solu-
tion can adversely affect the corrosion/oxida-
tion resistance, strength, working temperature 
(consequence of artificial reduction of melting 
point in interdendritic spaces) and formability 
in a warm, and can cause undesired phases due 
to segregation [6, 7]. Thus, by means of homo-
genisation annealing, the formability of bars, 
ingots and other cast semi-finished products 
is improved; in this case, casted rods made of 
aluminium alloys, since they have non-homoge-
neously distributed alloying elements through-
out the microstructure [8–10].
The uneven distribution of alloying elements 
inside the dendritic microstructure is a feature 
of high cooling rates. These differences increase 
with increasing cooling rates and greater differ-
ences in the composition between the melt and 
the solid phases at the beginning of crystallisa-
tion, which in some alloys can only be equated 
with long-term homogenisation as a result of 
solid-phase diffusion processes [11–13].
Owing to the non-equilibrium solidification, in 
the solid state, eutectic can be obtained, which 
according to the theoretical phase diagram 
should not form. Lowering the temperature 
at which incipient fusion started is so called 
a non-equilibrium solidus (NRS). In order to 
avoid local incipient fusion, each heat treatment 
must be carried out below the NRS temperature. 
Local incipient fusion may result in the forma-
tion of porosity resulting from the dissolution 
of non-equilibrium phases. The cracks formed 
during the forming can be the result of a molten 
eutectic phase that does not dissolve.
The degree of inhomogeneity is influenced by 
several different factors. The wider interval of 
solidification of the individual alloy in practical 
and theoretical aspects contributes to greater 
non-homogeneity. The increase in non-homo-
geneity is also influenced by the difference in 
the size of the solvent atoms and dissolved at-
oms, and their crystalline structure [5, 11].
The homogenisation annealing of cast struc-
tures to improve the formability was developed 
on the basis of empirical methods for determin-

Analysis of Chemical Composition Homogeneity in the Cross-section of the Rods Produced from Alloys of 6xxx Group
141
ing the time and temperature of the annealing. 
One of the determining factors is diffusion. In 
the empirical determination of the time and 
temperature of the annealing, the diffusivity of 
the local chemical composition must be taken 
into account. The diffusion of individual parti-
cles can be used to approximately determine 
the diffusion time, for which the following ex-
pression (1) can be used: [8, 10].
     ~
𝑥𝑥 2
𝐷𝐷 
 (1)
In this equation x is the diffusion path and rep-
resents half of the space between the secondary 
dendritic arms. Therefore, the process of ho-
mogenisation is more effective if the grains are 
smaller , since the elements need to take a short-
er path. D represents the diffusivity given in the 
following equation, whereas D
0
 represents dif-
fusion constant; Q is the activation energy for 
the diffusion; R is a gas constant and T is the 
temperature at which diffusion takes course.
    𝐷𝐷 = 𝐷𝐷 0
exp ⁡ (
− 𝑄𝑄 𝑅𝑅𝑅𝑅
)  (2)
According to this equation, the temperature has 
an exponential influence on the diffusion and 
consequently also on the time and tempera-
ture of homogenisation. By homogenisation 
annealing, only micro-segregation can be in-
fluenced. By the solidification of large castings, 
macro-segregations may occur, which may also 
be one metre high and could not be affected by 
homogenisation annealing [11].
In Table 1, the calculation of the diffusion co-
efficients of the various elements and the time 
needed at the certain temperature at which 
the element travels 50 m m (the hypothetical 
half-distance between the secondary dendritic 
arms) are given. Table 1 shows that the time 
drastically reduces with the rising temperature. 
Among the selected elements, the longest diffu-
sion times are for manganese, where at a tem-
perature of 600°C, the homogenisation anneal-
ing should last as much as for 567.3 h. Among 
other elements, only iron is also more difficult, 
which requires 21.6 h at the same temperature, 
while for other elements, the diffusion at a dis-
tance of 50 m m takes place in 2.2 h (Cu), 2.1 h 
(Al – self – diffusion), 0.7 h (Si), 0.5 h (Mg) and 
0.3 h (Zn) [14–17].
Table 1: Diffusion of elements in aluminium at temperatures 
550, 600 and 650°C at a distance of 50 mm [14–17].
Element T [°C] D [cm
2
/s] t [h]
Al
550 9.64E-10 7.2
600 3.32E-09 2.1
650 9.98E-09 0.7
Fe
550 6.70E-11 103.6
600 3.22E-10 21.6
650 1.30E-09 5.3
Si
550 3.21E-09 2.2
600 1.04E-08 0.7
650 2.95E-08 0.2
Mg
550 4.30E-09 1.6
600 1.31E-08 0.5
650 3.55E-08 0.2
Mn
550 2.01E-12 3461.6
600 1.22E-11 567.3
650 6.14E-11 113.1
Cu
550 9.83E-10 7.1
600 3.15E-09 2.2
650 8.88E-09 0.8
Zn
550 7.30E-09 1.0
600 2.00E-08 0.3
650 4.92E-08 0.1
Owing to all the factors listed earlier, which 
influence the quality of the production of cast 
rods, the process of homogenisation and fur-
ther processing of rods, two cross-sections of 
the rods from two different alloys of the 6xxx 
group, were analysed in this study. From the 
cross-sections of the rods, samples for differen-
tial scanning calorimetry (DSC) were taken at 
three locations in order to determine the effect 
of inhomogeneity on the DSC curve. The sam-
ples after the DSC analysis were, furthermore, 
metallographically prepared and microstruc-
ture was analysed, where the actual chemical 
composition was analysed using a scanning 
electron microscope (SEM) and an energy dis-
persion spectrometer (EDS).

Vončina M., Cvahte P ., Kračun A., Balaško T., Medved J. RMZ – M&G | 2019 | Vol. 66 | pp. 139–148
142
Materials and Methods
Based on the chemical composition of in-
vestigated alloys, which correspond to the 
EN AW-6008 and EN AW-6060 standards given 
in Table 2, a simulation of the thermodynami-
cally non-equilibrium solidification according 
to Scheil was performed using the Thermo-Calc 
software and the TCAL6 database.
In addition, DSC analysis was performed in 
order to determine the temperature chang-
es and the thermal effects that occur during 
heating/melting and cooling/solidification of 
the investigated alloys. Experiments were car-
ried out using the STA Jupiter 449C device from 
Netzsch by placing two identical corundum 
crucibles on the platinum sensor. In one cruci-
ble, the investigated sample, and in the other, 
a comparative (inert) sample was placed. The 
Table 2: Chemical composition of investigated alloys according to EN-AW standards in wt.%.
Alloy Si Fe Cu Mn Mg Cr Zn Ti V Al
6008 0.50–0.90 0.35 0.30 0.30 0.40–0.70 0.30 0.20 0.10 0.05–0.20 Rest
6060 0.30–0.60 0.10–0.30 0.10 0.10 0.35–0.60 0.05 0.15 0.10 – Rest
system was heated in a furnace according to 
the pre-programmed temperature program up 
to 720°C. At this temperature, it was kept for 
10 minutes. Heating and cooling stages were 
carried out at a constant rate of 10 K/min. The 
test was performed in a protective atmosphere 
of argon Ar 6.0. During the measurement, the 
apparatus measured the temperature, the 
difference in temperatures between the in-
vestigated and the comparative samples and 
the time. DSC analysis was carried out on cast 
samples taken from the centre, on D/4 and on 
the edge of the cross-section of the rod. The 
samples were cut from the cross-section of the 
rod and turning at a diameter of 4.5 mm and a 
height of 4 mm, which were inserted into the 
device where analysis was performed.
After the measurements, the heating and cool-
ing DSC curves were plotted; the characteristic 
temperatures were determined from heating 
and cooling DSC curves, and the influence of the 
sampling site on the characteristic tempera-
tures was analysed. After the DSC analysis, the 
samples were metallographically prepared and 
photographed using a BX61 light microscope 
with the purpose of analysing the influence of 
the sampling site from the cross-section of the 
rod on the formation and distribution of mi-
crostructural components. Furthermore, using 
the SEM Jeol JSM-7600F and EDS analyzer NCA 
Oxford 350 EDS SDD, the chemical composition 
of all samples after DSC analysis was analysed, 
and the homogeneity of the chemical composi-
tion in the intersection of the rod was analysed.
Results and Discussion
Figure 1a shows the calculated cooling curve 
of the alloy EN AW-6008 (Scheil’s model), with 
the dotted line showing the course of equi-
librium solidification. In this alloy, according 
to the calculation, in the microstructure, the 
primary α-Al, eutectic α-Al + Al
15
Si
2
M
4
 and eu-
tectic α-Al + Al
15
Si
2
M
4 
+ Al
9
Fe
2
Si
2
 phases can 
be expected, while at a lower temperature 
(approximately 568°C), the eutectic phases 
Al
18
Fe
2
Mg
7
Si
10 
and Mg
2
Si can solidify. Non-equi-
librium solidification begins at 654°C and ends 
at 558°C. In the following, the Scheil’s model of 
non-equilibrium solidification taking into ac-
count the large diffusion coefficients of the el-
ements of silicon and magnesium is calculated 
(Figure 1b). In this case, only three phases are 
obtained: α-Al, eutectic α-Al + Al
15
Si
2
M
4
 and eu-
tectic α-Al + Al
8
Fe
2
Si. The solidification starts at 
T
L
 = 654°C and ends at T
S
 = 603°C.
Figure 2 shows the calculated cooling curve 
of the alloy EN AW-6060 (Scheil’s model). In 
this alloy, the primary crystals of α-Al, eutectic 
α-Al + Al
13
Fe
4
 and eutectic α-Al + Al
13
Fe
4
 + A l
8
Fe
2
Si 
can be found in the microstructure; the phase 

Analysis of Chemical Composition Homogeneity in the Cross-section of the Rods Produced from Alloys of 6xxx Group
143
Figure 2: The cooling curve of the non-equilibrium solidification of the alloy EN AW-6060 without considering the diffusion (a) 
and taking into account the larger diffusion coefficients of the elements of silicon and magnesium (b).
Al
8
Fe
2
Si is transformed into the phase Al
9
Fe
2
Si
2
; 
also at a lower temperature, the eutectic phases 
Al
18
Fe
2
Mg
7
Si
10
 and Mg
2
Si can solidify. Non-equi-
librium solidification begins at 656°C and ends 
at 557°C. Figure 2b shows Scheil’s model of 
non-equilibrium solidification taking into ac-
count the large diffusion coefficients of sili-
con and magnesium. In this case, only three 
phases are obtained in the non-equilibrium 
curve: α-Al, eutectic α-Al + Al
13
Fe
4
 and eutectic 
α-Al + Al
13
Fe
4
 + Al
8
Fe
2
Si. The solidification starts 
at T
L
 = 656°C and ends at T
S
 = 616°C.
At the heating DSC curve, the Al
3
Ti and AlMg-β 
phases at the temperature of 233.2°C and 
282.4°C, respectively, presumably precipitate 
(Figure 3b), which was verified by thermo-
dynamic calculations/simulations of equi-
librium solidification and is a consequence 
of the supersaturated solid solution of the 
pre-hardened alloy. At 601.0°C, the eutectic 
α-Al + Al
8
Fe
2
Si melts, which represents a sol-
idus temperature, and at a temperature of 
609.6°C, the eutectic α-Al + Al
15
Si
2
M
4
 melts with 
respect to the Scheil’s calculation in Figure 1. 
Furthermore, at 646.8°C, melting of primary 
Figure 1: The cooling curve of the non-equilibrium solidification of the alloy EN AW-6008 without considering the diffusion (a) 
and taking into account the larger diffusion coefficients of the elements of silicon and magnesium (b).

Vončina M., Cvahte P ., Kračun A., Balaško T., Medved J. RMZ – M&G | 2019 | Vol. 66 | pp. 139–148
144
α-Al crystals is observed. During cooling, at a 
temperature of 648.6°C, the primary α-Al so-
lidifies; at a temperature of 599.0°C, eutectic 
α-Al + Al
15
Si
2
M
4
 and at a temperature of 572°C, 
eutectic α-Al + Al
8
Fe
2
Si. At 551.8°C, most like-
ly the Si
2
V eutectic phase solidifies (named as 
CrSi
2
 in the TC calculation).
Similar transitions are also observed on DSC 
curves of samples taken from the centre and 
edge of the cross-section of the rod, except 
that the temperatures slightly differ (Figure 3a 
and c). When comparing the curves, distinct 
differences are observed, which probably sug-
gests an inhomogeneous chemical composition 
in the cross-section of the rod (Figure 4). This 
is also confirmed by microstructural images 
after DSC analysis at various sites. The density 
of microstructural components is much higher 
Figure 3: Heating (blue) and cooling (green) DSC curves of the samples 6008_centre (a), 6008_D/4 (b) and 6008_edge (c) with 
marked characteristic temperatures and corresponding microstructure images.

Analysis of Chemical Composition Homogeneity in the Cross-section of the Rods Produced from Alloys of 6xxx Group
145
Figure 4: Comparison of heating (a) and cooling (b) DSC curves of EN AW-6008 alloy from different places of the rod: centre 
(blue), D/4 (green) and edge (red).
Figure 5: Heating (blue) and cooling (green) DSC curves of the sample 6060_centre (a), sample 6060_D/4 (b) and sample 6060_
edge (c) with marked characteristic temperatures and corresponding microstructure images.

Vončina M., Cvahte P ., Kračun A., Balaško T., Medved J. RMZ – M&G | 2019 | Vol. 66 | pp. 139–148
146
in the sample 6008_centre than in the sample 
6008_edge, whereas the distribution of micro-
structure phases is most uniform in the sample 
6008_D/4.
Figure 5 shows the heating and cooling DSC 
curves of samples from the EN AW-6060 al-
loy taken at three different locations with the 
accompanying microstructural images. At 
574.5°C, the eutectic α-Al + Al
8
Fe
2
Si begins to 
melt (according to the Scheil’s calculation in 
Figure 2b), which represents the solidus tem-
perature, and at a temperature of 624.1°C, the 
eutectic α-Al + Al
13
Fe
4
 melts. Furthermore, at 
642.1°C, the melting of the primary crystals of 
α-Al is observed. On the basis of the TC calcu-
lations of the equilibrium solidification, it can 
be concluded that the heating DSC curve leads 
to the precipitation of the phases Al
15
Si
2
M
4
 and 
Mg
2
Si at a temperature of 242.4°C and 371.2°C, 
respectively. During cooling, the primary 
α-Al (liquidus) solidifies at a temperature of 
649.7°C and eutectic with Fe phase (Al
13
Fe
4
 or 
Al
8
Fe
2
Si) solidifies at a temperature of 602.8°C, 
depending on the ratio between Fe and Si. Sim-
ilar changes are also observed on DSC analyses 
of samples taken from the centre (Figure 5a) 
and the edge (Figure 5c) of the cross-section 
of the rod, except that the temperatures differ 
slightly from one another. When comparing the 
heating (Figure 6a) and cooling (Figure 6b) of 
the DSC curves, it is observed that the curves 
are generally very similar, which indicates bet-
ter homogeneity of the chemical composition 
across the cross-section of the rod. The higher 
homogeneity of the chemical composition and, 
consequently, of the microstructural compo-
nents indicated by the results of the DSC anal-
ysis was confirmed also by the microstructural 
images shown next to the corresponding DSC 
analysis.
Figures 7 and 8 show the results of the EDS 
analysis on the samples after the DSC experi-
Figure 6: Comparison of heating (a) and cooling (b) DSC curves of EN AW-6060 alloy from different places of the rod: centre 
(blue), D/4 (green) and edge (red).
Figure 7: EDS analysis of samples from the alloy EN AW-6008 
taken from the cross-section of the rod at D/4, centre and edge 
after the DSC analysis.
Figure 8: EDS analysis of samples from the alloy EN AW-6060 
taken from the cross-section of the rod at D/4, centre and edge 
after the DSC analysis.

Analysis of Chemical Composition Homogeneity in the Cross-section of the Rods Produced from Alloys of 6xxx Group
147
ments confirming the preliminary conclusions; 
however, only the fluctuation of certain chem-
ical elements is presented since the actual 
chemical composition of the investigated alloys 
could not be revealed. It can be seen that the 
chemical composition is not homogeneous in 
the cross-section of the cast rod. The largest 
deviations in the EN AW-6008 alloy are found 
in a silicon concentration, which varies by more 
than 0.5 wt.%. Minor deviations are also found 
in concentrations of magnesium, vanadium, 
manganese and iron, which can be eliminated 
by appropriate homogenisation annealing.
Minor fluctuations in the chemical composi-
tion are shown by EDS analysis of the alloy 
EN AW-6060 (Figure 8), which was assumed 
already after the DSC analysis, where the DSC 
curves are very similar. The concentrations of 
magnesium, silicon, manganese and iron are 
slightly increased from the centre to the edge. 
EN AW-6060 alloy rods are fairly homogeneous 
in chemical composition already in the cast 
state.
Conclusion
The aim of this investigation was analysis of 
chemical composition homogeneity in the 
cross-sections of the rods produced from al-
loys of the 6xxx group. DSC analysis indicated 
non-homogeneity of the experimental alloys, 
whereas four reactions in case of EN AW-6008 
alloy and two reactions in case of EN AW-6060 
alloy could be expected, which corresponds 
to the Scheil’s non-equilibrium calculations, 
where larger diffusion coefficients of the ele-
ments of silicon and magnesium were taken 
into account.
On the basis of the results presented earlier, it 
can be concluded that the alloy EN AW-6060 
is already quite homogeneous in the cast state 
through the cross-section of the rod. The con-
centration of some elements slightly increases 
from the centre to the edge.
From the results of the analysis of the cross-sec-
tion of the rod from the EN AW-6008 alloy, it is 
evident that the chemical composition is not 
homogeneous in the cross-section of the cast 
rod. The greatest deviations are observed in 
the concentration of silicon, which also fluctu-
ates by more than 0.5 wt.%. Minor deviations 
are also found in concentrations of magnesium, 
vanadium, manganese and iron, which can be 
eliminated by appropriate homogenisation an-
nealing.
Acknowledgements
The work was co-financed by the Republic of 
Slovenia; the Ministry of Education, Science 
and Sport and the European Regional Devel-
opment Fund. The work was carried out in the 
framework of the project Modelling of thermo-
mechAnical pRocessing of The alumINium al-
loys for high quality products (MARTIN, Grant 
No.: C3330-18-952012).
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