M. PUCHNIN et al.: USE OF THE ABI TECHNIQUE TO MEASURE THE MECHANICAL PROPERTIES ...
247–252
USE OF THE ABI TECHNIQUE TO MEASURE THE
MECHANICAL PROPERTIES OF ALUMINIUM ALLOYS: EFFECT
OF CHEMICAL COMPOSITION ON THE MECHANICAL
PROPERTIES OF THE ALLOYS
UPORABA TEHNIKE ABI ZA MERJENJE MEHANSKIH
LASTNOSTI ALUMINIJEVIH ZLITIN: VPLIV KEMIJSKE SESTAVE
NA MEHANSKE LASTNOSTI ZLITIN
Maxim Puchnin1, Oleksandr Trudonoshyn1,2, Olena Prach1,2,3
1Czech Technical University in Prague, Karlovo námìstí 13, 12135 Prague 2, Czech Republic
2National Technical University of Ukraine “KPI”, Polytechnichna str. 35, Build. 9, 03056 Kiev, Ukraine
3Technische Universität Darmstadt, Karolinenplatz 5, 64289 Darmstadt, Germany
maxim.puchnin@fs.cvut.cz
Prejem rokopisa – received: 2014-12-08; sprejem za objavo – accepted for publication: 2015-03-10
doi:10.17222/mit.2014.294
The effects of the chemical composition on the microstructure and mechanical properties were investigated using automated
ball-indentation tests, scanning electron microscopy and energy dispersive X-ray analysis. It was observed that the mechanical
properties change with the presence of the eutectic and varying excess content of elements. In this work, the
automated-ball-indentation (ABI) technique was compared with the standard mechanical tests. The ABI method is based on
controlled multiple indentations into a polished surface by a spherical indenter under load. The indentation depth is
progressively increased to the maximum, user-specified limit, with intermediate partial unloading. This technique allows to
measure the yield strength, stress-strain curve, strength coefficient and strain-hardening exponent. For all these test materials
and conditions, the ABI-derived results were in very good agreement with those obtained with the conventional, standard test
methods.
Keywords: Al-alloys, microstructure, mechanical properties, ABI tests
Vpliv kemijske sestave na mikrostrukturo in mehanske lastnosti je bil preiskovan z avtomatskim preizkusom vtiskovanja krogle,
z vrsti~no elektronsko mikroskopijo in z energijsko disperzijsko rentgensko analizo. Opa`eno je bilo, da se mehanske lastnosti
spreminjajo s prisotnostjo evtektika in s spreminjanjem vsebnosti prese`nih elementov. V prispevku je bila preverjena metoda
avtomatskega vtiskanja kroglice (ABI) z obi~ajnimi mehanskimi preizkusi. ABI metoda temelji na kontroliranih ve~kratnih
vtiskih kroglastega vtiska~a v polirano povr{ino. Globina vtiskov progresivno nara{~a do maksimalne, z uporabnikom dolo~ene
meje, s takoj{njo vmesno razbremenitvijo. Ta tehnika omogo~a merjenje meje plasti~nosti, krivulje napetost-raztezek,
koeficienta trdnosti in eksponenta napetostnega utrjevanja. Za vse pogoje preizku{anja materiala so dobljeni ABI rezultati
skladni z rezultati, dobljenimi iz obi~ajnih metod preizku{anja.
Klju~ne besede: Al-zlitine, mikrostruktura, mehanske lastnosti, ABI preizkusi
1 INTRODUCTION
The growing demand for more fuel-efficient and
ecological vehicles to reduce energy consumption and air
pollution is a challenge for the automotive and aircraft
industries. The characteristic properties of aluminum,
high strength-to-weight ratio, good formability, good
electrical mass conductivity, unique corrosion behavior
and recycling potential make it the essential material for
the applications such as fuel-efficient transportation
vehicles, building construction, and food packaging.1
Si in Al-alloys improves the corrosion resistance of
the alloys. An addition of Si to composites significantly
affects the diffusion of Mg and Si in an Al liquid. Also,
when Si is used together with Mg, they create heat-treat-
able alloys. An extra Si content in Al-Mg2Si-Si compo-
sites leads to an increase of the solidification range. The
aspect ratio of the eutectics and the size of primary
particles decrease with the increasing Si content in
Al-Mg2Si composites.2,3
Mg in Al-alloys increases the weldability, improves
the corrosion resistance and decreases the weight of
alloys. An addition of Mg to aluminium alloys can in-
crease the hardness and strength of the materials.4 An
extra amount of Mg in the Al-Mg2Si system moves the
eutectic point to a lower Mg2Si concentration. Several
authors5–8 maintain that an excess of Mg in Al-Mg2Si
alloys can promote the formation of primary Mg2Si. It
also shows that increasing the Mg addition decreases the
volume fraction of the -Al matrix and increases the
volume fraction of the Al-Mg2Si eutectic.
Fe is the most common impurity found in Al. Fe re-
duces the grain size of an alloy, but decreases its hard-
ness and strength, and also increases the brittleness. Mn
improves the corrosion resistance and decreases the
negative effect of Fe.9,10
Materiali in tehnologije / Materials and technology 50 (2016) 2, 247–252 247
UDK 669.715:620.47:620.172 ISSN 1580-2949
Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 50(2)247(2016)
The main objective of this paper is to investigate the
influence of the chemical composition on the mechanical
properties and structures of Al-alloys.
The determination of the mechanical properties of
materials with non-conventional techniques has been an
active area of research for a long time. Among some
non-destructive methods for determining the mechanical
properties of materials, a semi-destructive type of test-
ing, called automated ball indentation (ABI), has been
developed. The automated-ball-indentation technique is
used to measure material properties when a tensile test
cannot be applied: in welded parts with a continuous
property variation, in brittle materials with an unstable
crack growth during preparation and specimen testing, in
samples with a high porosity and in the parts of the
present structural use.11,12
2 MATERIALS AND METHODS
The chemical compositions of the evaluated alloys
are shown in Table 1 and Figure 1.
All the alloys were prepared in an electric-resistance
furnace using graphite crucibles. High-purity Al
(A99.997), AlMg50, AlSi25 and AlMn26 were used as
master alloys. The melt with a temperature of 720
°C ± 5 °C was being degassed under an argon atmo-
sphere for 10 min.
Hardness was measured using a Brinell-hardness
testing machine (EMCOTEST M4C ) with a ball dia-
meter of 2.5 mm and a load of 62.5 kg; where the load
time was 10 s. Microhardness tests were performed on a
polished non-etched specimens using a LECO M-400-
G1 microhardness tester, HV0.05 with the standard
indentation time.
Tensile tests were performed using a testing machine
(INSTRON 5582, USA) according to the EN ISO 6892-1
standard. Tensile samples were also prepared according
to this standard.
Indentation tests were performed with a special
device (patent CZ 304637 B1), which is capable, due to
its design, of continuous recording of the load and inden-
tation depth of the used indenter. The system includes a
recording device, an analog-to-data converter, a PC with
software, and an Instron 5582 tensile-testing machine as
the force-producing mechanism. The maximum load
indentation was 2.5 kN and the indenter diameter was 5
mm. Plane-parallel samples were used for the ABI
testing.
M. PUCHNIN et al.: USE OF THE ABI TECHNIQUE TO MEASURE THE MECHANICAL PROPERTIES ...
248 Materiali in tehnologije / Materials and technology 50 (2016) 2, 247–252
Table 1: Nominal composition of alloys, in mass fractions (w/%) (Al–bal.)
Tabela 1: Nominalna sestava zlitin, v masnih dele`ih (w/%) (Al-ostalo)
Alloys Mg Si Mn Fe Ti Cu Zn Comment
AlMg6Mn (M3) 6.0 0.4 0.6 0.3 0.1 0.1 0.1 Al-1Mg2Si-5Mg
AlMg7SiMn (MS1) 7.0 1.0 0.6 0.02 0.1 0.05 0.05 Al-3Mg2Si-5Mg
AlMg7Si2Mn (MS2) 7.0 2.0 0.6 0.02 0.1 0.05 0.05 Al-6Mg2Si-3Mg
AlMg5Si2Mn (M59) 5.0 2.0 0.6 0.02 0.1 0.05 0.05 Al-6Mg2Si-1Mg
AlMg7Si3Mn (MS3) 7.0 3.0 0.6 0.02 0.1 0.05 0.05 Al-9Mg2Si-1Mg
AlMg7Si4Mn (MS4) 7.0 4.0 0.6 0.02 0.1 0.05 0.05 Al-10.5Mg2Si-0.5Si
AlMg7Si5Mn (MS5) 7.0 5.0 0.6 0.02 0.1 0.05 0.05 Al-10.5Mg2Si-1.5Si
AlSi7Mg (S1) 0.3 6.9 0.02 0.2 – 0.05 0.05 Al-7Si
Figure 1: Equilibrium-phase diagrams
Slika 1: Ravnote`ni fazni diagrami
3 RESULTS AND DISCUSSION
3.1 Microstructure investigation
Figure 2 presents the polished microstructures of the
samples. The microstructures of all the samples consist
of primary Al grains (the light areas) and the
(Al)+(Mg2Si) eutectic (grey). The preferential morpho-
logy of -Al is a globular-rosette morphology and Al
grains are surrounded by eutectic colonies. The
(Al)+(Mg2Si) eutectic has a lamellar morphology. Pri-
mary Mg2Si crystals have a regular polyhedral shape and
are located in the centers of the eutectic colonies.
3.2 Element distribution in a-Al grains
The -Al matrix of the Al-Mg-Si-Mn alloys contains
Mg, Si and Mn. It is known that the solubility of Mg in
Al amounts to 1.4 % and the solubility of Si is 0.4 % at
room temperature.10
In the investigated alloys, the Mg and Si contents in a
solid solution change with an alteration of the Mg/Si
ratio in the alloys (Table 2). The stoichiometric compo-
sition of Mg2Si is 66.7 % of amount fractions of Mg and
33.3 % of amount fractions of Si (the Mg/Si at. ratio is
2.0, and its weight ratio is 1.73:1). The Mg content is
considered to be in excess when the ratio is more than 2,
and the Si content is in excess when the ratio is less than
2. For all the alloys, the Mn content in the -Al solid
solution is ~0.5 % of mass fractions. The existence of an
insignificant peak of oxygen in the EDX spectrum is
explained with the tendency of Al and Mg silicides to
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Materiali in tehnologije / Materials and technology 50 (2016) 2, 247–252 249
Figure 2: Microstructures of as-cast state of Al-Mg-Si-Mn alloys: a) AlMg6Mn (M3), b) AlMg7SiMn (MS1), c) AlMg7Si2Mn (MS2),
d) AlMg7Si3Mn (MS3), e) AlMg7Si4Mn (MS4), f) AlMg7Si5Mn (MS5), (according to the Table 1). The names of phases: 1. Matrix of -Al,
2. Primary Mg2Si phase, 3. Eutectic of Al-Mg2Si, 4. -Al15(Mn,Fe)3Si2, -Al5(Mn,Fe)Si, 5. -Al4Si2(Mn,Fe).
Slika 2: Mikrostruktura zlitin Al-Mg-Si-Mn, v litem stanju: a) AlMg6Mn (M3), b) AlMg7SiMn (MS1), c) AlMg7Si2Mn (MS2),
d) AlMg7Si3Mn (MS3), e) AlMg7Si4Mn (MS4), f) AlMg7Si5Mn (MS5), (glede na Tabelo 1). Imena faz: 1. Osnovna -Al, 2. Primarna Mg2Si
faza, 3. Evtektik Al-Mg2Si, 4. Mn-faza Al6(Mn,Fe), -Al15(Mn,Fe)3Si2, -Al5(Mn,Fe)Si, 5. Si-Mn faza -Al4Si2(Mn,Fe)
Table 2: Average composition of -Al solid solution in Al-Mg2Si
alloys measured with EDX
Tabela 2: Povpre~na sestava trdne raztopine -Al v Al-Mg2Si zliti-
nah, izmerjena z EDX
Alloy Mg/Siratio
Chemical composition (w/%)
Mg Al Si Ti Mn Fe
MS1 (AC)
7.0
5.8 93.2 0.2 0.2 0.5 <0.1
MS1 (ST) 5.9 93.1 0.2 0.2 0.5 <0.1
MS1 (AA) 5.9 93.2 0.1 0.2 0.5 <0.1
MS2 (AC)
3.5
3.5 95.5 0.2 0.2 0.5 <0.1
MS2 (ST) 3.9 95.1 0.2 0.2 0.5 <0.1
MS2 (AA) 3.7 95.4 0.1 0.2 0.5 <0.1
MS3 (AC)
2.2
2.5 96.3 0.3 0.3 0.5 <0.1
MS3 (ST) 2.4 96.5 0.2 0.3 0.5 <0.1
MS3 (AA) 2.4 96.6 0.2 0.3 0.4 <0.1
MS4 (AC)
1.8
2.1 96.6 0.5 0.3 0.4 <0.1
MS4 (ST) 1.3 97.0 0.8 0.3 0.5 <0.1
MS4 (AA) 1.3 97.0 0.8 0.3 0.5 <0.1
MS5 (AC)
1.4
1.5 96.6 1.1 0.3 0.4 <0.1
MS5 (ST) 0.8 95.8 1.4 0.3 0.5 <0.1
MS5 (AA) 0.8 96.9 1.4 0.3 0.5 <0.1
AC – as cast state, ST – after solution treatment (570 °C, 60 min), AA
– after artificial aging (at the point of maximum mechanical proper-
ties)
oxidation. The average composition of the -Al matrix for
all the samples is presented in Table 2.
The solution treatment increases the concentration of
Mg and decreases the concentration of Si (Table 2) in
the solid solutions in the MS1 and MS2 alloys (the alloys
with an excess Mg concentration). The artificial aging
leads to a further reduction in the concentration of Si (it
is connected with a small amount of Si in the alloys and
the tendency of Mg to form the Mg2Si compound), but
the concentration of Mg is back to the initial values.
The situation is different in the MS3, MS4, MS5
alloys. During the solution treatment, taking 60 min, the
amount of Mg reduces and the amount of Si increases in
these alloys. The increase in the concentration of Si in
the solid solution is connected with the dissolution of
Mn-containing phases. Aging does not significantly
change the chemical composition of -Al (Table 2).
3.3 Mn- and Si-containing phases
Due to a poor solubility, Fe with Si and Al in the
Al-Mg-Si alloys constitute acicular-shaped intermetallic
inclusions, which reduce the mechanical properties of
the alloys. The investigated alloys are additionally doped
by 0.6 % Mn to neutralize the negative effect13–15 of the
Fe-containing phase. As it is shown by other studies, an
addition of 0.6 % of mass fraction of Mn in the alloy
with a nominal composition of Al-7Mg-3Si improves its
mechanical properties. Thus, the tensile strength and
yield strength of the alloy with the Mn addition increase
on average by 30 %.
Some authors13 reported that in the alloy with a nomi-
nal composition of Al-7Mg-5Si (w/%), the Al-Mg2Si
eutectic and Al-Si eutectic are formed. However, the
Al-Si eutectic was not detected in the alloy with a nomi-
nal composition of Al-7Mg-5Si-Mn (Figure 2f). There-
fore, the excess Si with Mn and Fe form several types of
the Mn-phase in the submitted alloys.
The morphologies of all the types of the Mn-contain-
ing phases observed in the MS-series are shown in
Figure 2. These phases can be identified as Al6(Mn,Fe),
-Al15(Mn,Fe)3Si2, -Al5(Mn,Fe)Si, -Al4(Mn,Fe)Si2.
The first two types are found in the alloys with the ratio
of Mg/Si greater than 2 (M3, MS1, MS2, MS3, M59).
Phases  and  are found in the alloys with the ratio of
Mg/Si lower than 2 (MS4, MS5). The -phase is un-
stable and it disintegrates during the heat treatment.15–17
3.4 Eutectic
The EDX spectra of the lamellas excluding Al from
the quantification showed a composition very close to
the stoichiometry of Mg2Si. The EDX spectra of inter-
lamellar spacing show high concentrations of Mg and Si.
With the increase in Mg and Si, the Al-Mg2Si eutectic
volume fraction grows bigger.18
With the addition of extra Mg into the Al-Mg2Si
system, the eutectic point moves towards the corner with
a lower Mg2Si concentration and the volume of the
Al-Mg2Si eutectic increases.
With the addition of extra Si into the Al-Mg2Si
alloys, the eutectic point moves to a higher Al concen-
tration and the volume of the Al-Mg2Si eutectic in-
creases. In the AlMg7Si5Mn alloy (with 1.5 % of mass
fractions of excess Si and 0.6 % of mass fractions of Mn)
the volume fraction of the Al-Mg2Si eutectic reaches its
maximum.
3.5 Reproducibility of the results of classical tests and
ABI tests
Figure 3 represents the dependencies of the inden-
tation-depth load, recorded in the ABI study. They show
how the material behaves in the research process, which
consists of three parts: the load, the holding at the
maximum force and the unloading. The growing part of
the curve describes the process of loading. This process
has elastic and elastic-plastic sections.19 Then, after the
holding at the maximum force for 10 s, the unloading
process begins. The waning part of the curve describes
the process of unloading. The point where the curve
intersects with the x-axis corresponds to the plastic
indentation depth (hp). The difference between the plastic
depth and the depth of the maximum load (hmax) corres-
ponds to the elastic depth (hs).
For the results validation, the data obtained with the
ABI method were compared with the data obtained with
the classical methods (Table 3).
The hardness was calculated with Equation (1) and
Equation (2)20 was used to determine the tensile strength
(Rm):
HB
P
Dh
=
π
(1)
R c HBm = ⋅ (2)
where: HB – Brinell hardness, P – load (kN) (Figure 3),
D – diameter of indenter (mm), h – indentation depth
(mm) (Figure 3), ñ – coefficient of uncertainty for the
presented series of alloys with a value of 2.8.20
M. PUCHNIN et al.: USE OF THE ABI TECHNIQUE TO MEASURE THE MECHANICAL PROPERTIES ...
250 Materiali in tehnologije / Materials and technology 50 (2016) 2, 247–252
Figure 3: ABI indentation curves
Slika 3: ABI krivulje vtiskovanja
The methodology from the reference20, Equations (3)
and (4), was used to determine the yield strength (Rp0.2):
R c HM
c P
ap0.2
= ⋅ =
⋅
π 2
(3)
a Dh h= − 2 (4)
where: c – coefficient of uncertainty (2.8), HM – Meyer
hardness, a – contact radius (mm).
The differences between the two curves given in the
diagrams (Figure 3) may be related to the following
parameters taken into account in Equation (1):
1. The difference in the value of the load (P), which
leads to a change in the indentation depth.
2. The difference in the hardness of the materials (HB).
Figure 3 shows the indentation curves of the alloys
with a difference in the amount of one component (Mg,
Si, Mg2Si). The results of the ABI tests are shown in
Table 3.
The calculation of the standard deviation shows that
the hardness value is determined with a sufficiently high
accuracy. The average deviation is about 2–3 %. The
tensile strength (defined by the HB values) has a good
accuracy (its average deviation is 3–5 %).
The values of the average standard deviation of the
yield strength are quite high (9–16 %), but in some tests
the accuracy is 1 %. This can be explained in the
following manner: the load, at which the deformation is
detected in the track (0.2 %) is about 100 N and the
measurement device determines the load with an accur-
acy of 24 N – 50 N. This is sufficient for the deter-
mination of the total hardness, but it is not enough for
the determination of the hardness at the load of P0.2. It is
planned to increase the accuracy of the determination of
this and other parameters.
3.6 Influence of the chemical composition on the me-
chanical properties
As it can be seen from Table 3, the mechanical pro-
perties of the cast Al-Mg2Si alloys do not increase with
the growth of the Mg content (Figure 3b, alloys MS2
and M59 – alloys with similar values of Mg2Si and diffe-
rent values of Mg). Similar results of the Mg behavior in
Al-alloys were obtained in another study.21
An analysis of the literature data3,13 showed that the
mechanical properties of the Al-Mg2Si-Si alloys with an
increased amount of Si are improved. However, in these
works the mechanical properties are given after the heat
treatment of the alloys. In the considered series of alloys,
extra Si with Mn forms a metastable acicular-shaped
-Al4(Mn,Fe)Si2 phase, which deteriorates the properties
of the alloys in the as-cast state, and this phase dissolves
during the homogenization process.
As can be seen in Table 3, the hardness and the
tensile strength of the cast Al-Mg2Si alloys can relate to
the size and morphology of the eutectic and primary
Mg2Si phase (M3 and MS1, M59 and MS3 are alloys
with similar values of Mg and different values of Mg2Si).
Hence, the mechanical properties grow with the
increasing volume fraction of Mg2Si. Similar results
were obtained in a reference study.6
4 CONCLUSIONS
The comparison of the results obtained with classical
and ABI methods shows the following:
• The differences in the values of the hardness and
tensile strength, obtained with different methods, do
not exceed 5 % (with the standard error for such
measurements of 10 %).
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Materiali in tehnologije / Materials and technology 50 (2016) 2, 247–252 251
Table 3: Comparison of the results obtained with classical methods and ABI method
Tabela 3: Primerjava dobljenih rezultatov s klasi~nimi metodami in z ABI metodo
State Method S1 M3 M59 MS1 MS2 MS3 MS4 MS5
As-cast
state
HB, ABI 72 65.0 82.3 83.6 83.9 89.4 70.0 66.2
HB* 75 65.0 81.0 84.0 86.8 87.8 71.1 69.0
Rp0.2, (MPa), ABI 180.2 145.6 166.4 194.1 134.4 223.9 145.5 124.8
Rp0.2, (MPa)* 182.5 130.0 155.5 169.4 155.3 203.5 137.9 123.5
Rm, (MPa), ABI 201.6 179.5 226.1 229.5 230.5 245.6 192.4 182.0
Rm, (MPa)* 205.1 180.0 219.9 199.4 223.1 239.8 185.6 163.5
ST 1 h,
570 °C
HB, ABI – – 73.0 79.1 70.5 73.1 71.1 78.7
HB* – – 71.0 77.5 69.6 73.2 71.1 75.5
AA
(1 h,
570 °C +
1.5 h,
75 °C)
HB, ABI 90.0 – 93.6 83.6 80.9 99.5 100.4 107.3
HB* 90.0 – 96.1 82.2 79.6 100.7 101.9 113.7
Rp0.2, (MPa), ABI 194.1 – 155.4 194.1 145.6 179.2 224.0 233.0
Rp0.2, (MPa)* 171.9 – 175.3 174.2 164.2 200.6 227.1 200.8
Rm, (MPa), ABI 243.0 – 257.1 229.7 222.4 273.1 275.8 294.7
Rm, (MPa)* 256.9 – 256.3 226.2 222.1 262.4 264.9 280.7
* – Classic methods
• The error of the yield-strength measurement is
greater than 10 % (and varies from 1 % to 16 %).
This problem can be solved by increasing the
sensitivity of the device at low values of the load.
• The analysis of the results of the hardness and tensile
tests shows the following:
• Excess Mg does not have a significant effect on the
mechanical properties of the alloys.
• Metastable -Al4(Mn,Fe)Si2 phases are formed in the
alloys with excess Si. This leads to a degradation of
the mechanical properties.
• The main strengthening phase in the as-cast state of
the studied alloys is the Al-Mg2Si eutectic.
Acknowledgments
The authors gratefully thank the Visegrad Fund and
DAAD for their support in the research. Also, the
authors would like to thank doc. Ing. Jirí Cejp, C Sc. and
doc. Ing. Jirí Janovec, C Sc. for their help with the
tensile tests, and Ing. Jakub Horník, Ph.D., for super-
vising the present investigations.
This work was supported by the Ministry of Educa-
tion, Youth and Sport of the Czech Republic, program
NPU1, the project with Nos. LO1207 and SGS13/
186/OHK2/3T/12 – Research on the influence of surface
treatment on the improvement of service life and
reliability of exposed water turbine’s components.
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