Materials Science & Engineering A 590 (2014) 416–422

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Structural and mechanical properties of ZnMgO nanoparticles

M. Tosun a, S. Ataoglu b,c, L. Arda d,n, O. Ozturk e, E. Asikuzun e, D. Akcan d, O. Cakiroglu f
a
Istanbul Technical University, Faculty of Mechanical Engineering, 34437, Gumussuyu, Istanbul, Turkey
b
Istanbul Technical University, Faculty of Civil Engineering, 34469, Maslak, Istanbul, Turkey
c
Istanbul Technical University, Earthquake Engineering and Disaster Management Institute, 34469, Maslak, Istanbul, Turkey
d
Bahcesehir University, Faculty of Arts and Sciences, Department of Mathematics & Computer Sciences, Ciragan Cad, Osmanpasa Mektebi Sok, 34349,
Besiktas, Istanbul, Turkey
e
Kastamonu University, Faculty of Arts and Sciences, Department of Physics, 37100, Kastamonu, Turkey
f
Hasan Ali Yucel Education Faculty, Istanbul University, 34452, Beyazit, Istanbul, Turkey

art ic l e i nf o a b s t r a c t

Article history: This study reports the effect of annealing temperature on the structure and mechanical properties of
Received 30 September 2013 Zn0.95Mg0.05O bulk samples by using digital Vickers microhardness tester, X-ray diffraction analysis,
Accepted 12 October 2013 scanning electron microscopy and electron dispersive X-ray measurements. The samples were prepared
Available online 31 October 2013
using Zn and Mg based alkoxed by the sol–gel technique and annealed at various temperatures (500, 600,
Keywords: 700 and 800 1C). Vickers microhardness, elastic modulus, yield strength and fracture toughness values of
Hardness measurement Zn0.95Mg0.05O bulk samples were separately calculated and compared with each other. The experimental
Mechanical characterization results of hardness measurements were analyzed using Meyer's law, Proportional Specimen Resistance
ZnMgO (PSR) and Elastic/Plastic Deformation (EPD) models and Hays–Kendall (HK) approach. Finally, it was seen
Sol–gel
that HK approach is the most successful model for the microhardness analysis of these materials.
Microhardness
& 2013 Elsevier B.V. All rights reserved.

1. Introduction optical properties of ZnMgO; however not enough can be found

about the mechanical properties which are relevant to the
The interest in ZnO and doped ZnO is increasing day by day strength of these materials.
because of their physical and electronic properties which have The mechanical properties are mainly due to interatomic bond-
been found to be promising for the technological applications such ing forces. In addition to this, the internal structure of the material
as magnetic memory devices, transparent conducting electrodes, and mechanical properties may be significantly improved with the
heat protecting windows, light emitting diodes (LED), gas sensors, internal structural modifications. As it is known, important para-
solar cells, laser systems, etc. [1–4]. ZnO has a direct bandgap of meters such as hardness, yield strength, elastic modulus, fracture
3.37 eV with excitonic energy of 60 meV in a semiconductor. It toughness and brittleness for the mechanical characterization of the
crystallizes in a hexagonal wurtzite structure with lattice para- materials change extremely with different doping [9–12]. The
meters of a ¼3.249 nm and c¼ 5.205 nm. determination of mechanical properties of ZnMgO is important in
When ZnO is doped, properties of ZnO are changed. One of the applications including window materials for display, solar cells,
these properties is the bandgap which can be controlled via liquid crystal displays and heat mirrors.
divalent substitution on the cation site. The bandgap decreases In this study, the hardness analysis have been carried out using
to approximately 3 eV by substituting Cd on Zn site, but, on the existing and widely used methods in the literature, Meyer's Law,
other hand, substituting Mg on Zn site increases the bandgap to the Proportional Sample Resistance and Elastic/Plastic Deforma-
4 eV and higher [5]. Mg doped ZnO semiconductors have been tion, Indentation-Induced Cracking (IIC) models and HK approach.
found to be promising candidates for solar cells, liquid crystal The aim of this work is to investigate the effect of temperature on
displays and heat mirrors. So, many researchers have prepared the mechanical properties of ZnMgO samples exposed to heat-
MgxZn1  xO bulk and films using various methods [6–8] due to treatment at different temperatures (500, 600, 700 and 800 1C).
their physical and electronic properties which show differences
according to the method used to prepare the samples. There have
been many publications written on the electrical, magnetic and 2. Experimental procedures

The systems, Zn0.95Mg0.05O, were prepared as polycrystalline

n
Corresponding author. Tel.: þ 90 212 3810323; fax: þ90 212 3810000. nanoparticle powders by the sol–gel technique. Zinc acetate dihy-
E-mail address: lutfi.arda@bahcesehir.edu.tr (L. Arda). drate (Fluka) and Mg 2,4 pentadionate (Alfa Easer) were precursor

0921-5093/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2013.10.024
 M. Tosun et al. / Materials Science & Engineering A 590 (2014) 416–422 417

materials. Methanol and acetyl acetone were used as solvents to

prepare clear homogenous solutions.
After weighing the appropriate amounts, the precursor materials
and solvents were all mixed thoroughly with a magnetic stirrer for
8 h at room temperature until a transparent solution was obtained.
The pH values of the solutions were measured by a standard pH
meter (ORION 3 Star). The concentrations of the solutions were
0.09 mol/l. Then, the solutions were removed from the solvent at
the room temperature using the magnetic stirrer. After that, the
powders were preheated at 400 1C for 10 min in air and were
grounded. Ground nanoparticles were pressed under a load of 10 t
for 10 min into disk shaped compacts with a thickness of 2 mm and
a diameter of 10 mm. Pressed samples were annealed at various
temperatures (500, 600, 700 and 800 1C) for 30 min in air.
Zn0.95Mg0.05O phase of pellet samples was identified by means Fig. 2. The XRD profile fitting resulting from the Rietveld analysis of ZnMgO.
of X-ray diffraction using Bruker D8 Advance model diffractometer
with Cu-Kα radiation (λ ¼1.5418 Å). Data for powder samples were Table 1
collected over the range 201o2θo901 in 0.21 2θ step, with an Particle sizes of the Zn0.95Mg0.05O nanoparticle at different
integration time of 0.5 s. Particle size and stoichiometry of pellets temperatures.
were ascertained using SEM (JEOL, JSM-5910LV). Chemical com-
Temperature (C1) D (nm)
position of samples was done by means of dispersive spectrometry
(EDS) in the SEM. Vickers microhardness measurements have been 500 14.35
made on the sample surfaces at room temperature using a digital 600 25.48
microhardness tester (SHIMADZU). The load was applied for 10 s 700 20.90
800 28.54
and varied in the range of 0.245–2.940 N. The indentations have
been made at different regions of the sample surfaces making sure
that the indentations do not overlap.
(100) and are indicated in Table 1. Fig. 3 shows the SEM micrograph of
the pressed powder samples. The particle sizes for the pressed
3. Results and discussion samples are in the range of 60–300 nm. This is an expected result
because of the agglomeration between the nanoparticles due to
ZnMgO samples were prepared by using the sol–gel technique. pressing. Agglomeration between nanoparticles is predominant as
The X-ray diffractions of the Zn0.95Mg0.05O samples at various seen in SEM image in Fig. 3. The composition of the Zn0.95Mg0.05O
temperatures (500, 600, 700, and 800 1C) for 30 min in the air are nanoparticle is investigated by EDS. EDS spectrum of Zn0.95Mg0.05O is
shown in Fig. 1. All the peaks belong to the hexagonal lattice of ZnO. seen in the inset of Fig. 3b. Zn and Mg peaks are clearly seen and the
But, many studies done on the magnetic, electrical and optical content of Zn and Mg are consistent with preparation of samples.
properties of ZnMgO exist, often with ambiguous and even contra-
dicting results. One of the key questions is whether the resulting 3.1. Vickers microhardness measurements
materials are indeed a single phase alloy of ZnMgO or not. So, XRD
results were examined by using Rietveld analysis applying the Five different loads (0.245, 0.480, 0.980, 1.96 and 2.940 N) are
MAUD program [13]. The analyses showed that the reflections applied to the samples to determine the Vickers microhardness
correspond to ZnO hexagonal wurthzite structure without second- values of the materials. It is necessary to take into consideration that
ary phases (Fig. 2) as seen in the previous study [7]. the indent should be pressed on different surfaces of the samples
The average particle size of Zn0.95Mg0.05O pellet samples were but traces should not overlap. Then, on the material's surface,
estimated from the data of full width half maximum (FWHM) in diagonals of the trace left by the indenter are read using the
the XRD spectrum using the Sherrer equation ½D ¼ Kðλ=Δθ cos θÞ, microscope. The relation between load/trace area and Vickers
where K is a constant (0.9), λ is the X-ray wavelength (0.15406 nm), Δθ hardness are calculated using the relation given below:
is the width of the line at the half-maximum intensity and θ is the half

of the diffraction angle. The average particle size was calculated for the F
H ν ¼ 1854:4 2 ðGPaÞ ð1Þ
highest 3 intense peaks of this sample at spectrum (101), (002) and d
where F is the applied load in N and d is the diagonal length of the
indentation mark in mm. In addition, values of the load-dependent
elastic modulus, E, yield strength, Y and fracture toughness, KIC were
calculated using Eqs. (2)–(4) given below for all samples
E ¼ 81:9635H ν ð2Þ

Hν
Y ð3Þ
3
pffiffiffiffiffiffiffiffiffi
K IC ¼ 2Eα ð4Þ
where α is the surface energy. The results are presented in Table 2.
If Table 2 is examined, it can be discerned that microhard-
ness values are dependent on the load applied by the indenter
(RISE: Reverse Indentation Size Effect). When different annealing
Fig. 1. XRD patterns of the Zn0.95Mg0.05O nanoparticle with various temperatures. temperatures are taken into consideration changes in microhardness
418 M. Tosun et al. / Materials Science & Engineering A 590 (2014) 416–422

Fig. 3. SEM micrographs of the Zn0.95Mg0.05O nanoparticle at (a) 600 1C with high magnification, (b) 600 1C with low magnification, (c) 800 1C with high magnification,
(d) 800 1C with low magnification, The inset shows the EDS spectrum of Zn0.95Mg0.05O nanoparticles at 600 1C.

Table 2 Application of more force may be needed for changing its shape if
Hv, E, Y and KIC load-dependent values of the samples. the material is tough. Thus, elastic modulus increases. KIC is
referred to as fracture toughness. However, it can also be called
Samples F (N) d (mm) Hv (GPa) E (GPa) Y (GPa) KIC (Pa/m1/2)
brittleness. As the hardness of the material increases so does its
500 1C 0.245 40.27 0.280 22.95 0.093  289.82
brittleness. Since E and Y values are dependent on the hardness,
0.490 54.04 0.311 25.49 0.103  305.44 the hardness increases in tandem with these. Increases in E and Y
0.980 73.40 0.337 27.62 0.112  317.95 values is the expected result since the hardness values increase
1.960 103.49 0.340 27.86 0.113  319.32 with the increase of temperature for all samples of ZnMgO (500,
2.940 126.06 0.344 28.19 0.114  321.21
600, 700 and 800 1C). The indentation marks and cracks are
600 1C 0.245 38.28 0.310 25.40 0.103  285.99
0.490 50.11 0.354 29.01 0.118  305.63 observed on the sample in Fig. 4. The cracks were formed in
0.980 70.91 0.368 30.16 0.122  311.63 median and one side of the sample under the indentation load of
1.960 98.74 0.374 30.65 0.124  314.15 o2.940 N.
2.940 120.34 0.377 30.90 0.125  315.43
Variations of Vickers microhardness values as a function of
700 1C 0.245 37.74 0.320 26.22 0.106  327.07
0.490 49.48 0.364 29.83 0.121  348.86
the applied load for the samples are shown in Fig. 5. It can be
0.980 69.14 0.382 31.31 0.127  357.41 seen from the curves in Fig. 5 that microhardness values
1.960 96.37 0.393 32.21 0.131  362.51 increase when the applied load is increased for all samples of
2.940 116.93 0.399 32.70 0.133  365.26 ZnMgO annealed at 500, 600, 700 and 800 1C. Microhardness
800 1C 0.245 37.20 0.330 27.04 0.110  215.66
values reach a plateau (saturation region) at around 1.5 N for all
0.490 41.03 0.381 31.22 0.127  231.73
0.980 65.41 0.425 34.83 0.141  244.76 the samples. That is, no matter how much load over 1.5 N is
1.960 90.16 0.447 36.63 0.149  251.01 applied to the material, changes in the microhardness value will
2.940 109.99 0.451 36.96 0.150  252.13 be insignificant. These indicate that the hardness value depends
on the applied load and there is a relation between the load and
size of the indenter. In this study, the hardness values increased
when the applied load is increased. This phenomenon is
values of these samples in relation to the load applied can be reported as the Reverse Indentation Size Effect (RISE) in the
perceived. It can additionally be recognized that the more the literature. This means that the smaller the indenter's load the
annealing temperature, the more the microhardness values for all smaller the hardness.
ZnMgO samples. RISE behavior was observed for all samples, i.e. Variation of microhardness according to load rises the question
increase in microhardness with increasing applied load. “what should be the real microhardness?” In the literature, the
Values of microhardness plus elastic modulus, yield strength different models for explaining the behavior of the Indentation
and fracture toughness are calculated as a function of the load and Size Effect (ISE) and RISE are presented. In this section, compar-
are listed in Table 2. These parameters are very important for the isons related to the hardness will be made using Meyer's Law, the
mechanical characterization of the materials. Elastic modulus is a PSR and EPD models, HK approach and IIC model. Investigations
measure of the elastic deformation of the material under the force. related to these models are given below.
 M. Tosun et al. / Materials Science & Engineering A 590 (2014) 416–422 419

Fig. 4. Vickers indentation marks on Zn0.95Mg0.05O.

Fig. 6. Variation of applied load ln F with diagonal ln d for the samples.

Fig. 5. Variations of microhardness with load for the samples.

Table 3
Best-fit results of experimental data according to Meyer's law.
3.2. Analyses and modeling
Samples nK ln A1K (GPa) Hv (GPa)
3.2.1. Meyer's law
It is the simplest method used to explain the ISE behavior and 500 1C 2.17  9.42 0.340–0.344
how the applied load is related to the size of the indenter 600 1C 2.14  9.18 0.374–0.377
700 1C 2.17  9.27 0.393–0.399
nK
F ¼ Ad ð5Þ 800 1C 2.10  8.79 0.447–0.451

where A is the standard hardness constant and superscript nK is

Meyer's number and is obtained from the curves fitted according developed by Li and Bradt [15]. This model is given as follows:
to the experimental data. And, it is also considered as a measure of
F
ISE behavior. If the value of nK is greater than 2 RISE however less ¼ α þ βd ð6Þ
than 2 ISE behavior was observed; if nK ¼2 the hardness is d
independent of the load that gives Kick's law (F¼A1Kd2) [12,14]. Here α and β values are calculated from (F/d)  d graph (Fig. 7).
Slope of the graph is proportional to nK and that of vertical The change in α value is related to the distribution of energy of the
intercept is proportional to A1K. nK values obtained from the slope surface cracks [16]. In PSR model, load-independent hardness
of the graph of the ln F–ln d are greater than 2 for all samples in values are calculated as
Fig. 6. Meyer's number greater than 2 for the samples analyzed
H PSR ¼ 1854:4β ð7Þ
confirms that the character of displacement behavior load-
dependent is in the form of the RISE behavior. These data are As can be seen from Table 4, α value is negative for all samples
summarized in Table 3. It can be said that the RISE behavior was showing RISE behavior. This case indicates that there is only plastic
observed for all samples based on the nK value obtained from the deformation in the samples showing the RISE behavior and no
slope of the graph of ln F–ln d. elastic. There was no elastic deformation for the loads applied.
There has not been a relaxation in the surface of the material after
3.2.2. PSR model the indenter has been dipped and removed. This causes a quantity
Proportional Specimen Resistance is a model used for the increase on the material hardness. β is a parameter that is used to
hardness analysis of materials having ISE behavior and was find the real hardness value.
420 M. Tosun et al. / Materials Science & Engineering A 590 (2014) 416–422

Table 5
Calculated load-independent Hv, Eo, Yo and KIC for the samples.

Samples Ho (GPa) Eo (GPa) Yo (GPa) KIC (Pa/m1/2) Hv (GPa)

500 1C 0.370 30.32 0.123  333.12 0.340–0.344

600 1C 0.402 32.94 0.134  325.67 0.374–0.377
700 1C 0.430 35.24 0.143  379.18 0.393–0.399
800 1C 0.463 37.94 0.154  255.45 0.447–0.451

Fig. 7. Plots of F/d versus d for the samples.

Table 4
Best-fit results of experimental data according to PSR model.

Samples β  10  4 (N/μm2) HPSR (GPa) α  10  3 (N/mm) Hv (GPa)

500 1C 2.00 0.370  1.83 0.340–0.344

600 1C 2.17 0.402  1.61 0.374–0.377
700 1C 2.32 0.430  2.04 0.393–0.399
Fig. 8. Plots of square root of applied loads versus diagonal length for the samples.
800 1C 2.50 0.463  0.86 0.447–0.451

Values transition to the plateau of the samples in Fig. 5 according Table 6

Best-fit results of experimental data according to EPD model.
to the Quinn and Quinn approach are far from the load-independent
hardness values calculated by PSR model. For this reason, it is clearly Samples A2 (N/mm2) de (mm) HEPD (GPa) Hv (GPa)
seen that PSR model is inadequate in determination the real
hardness values of the materials. In addition, using value of HPSR 500 1C 0.0142  0.07 0.373 0.340–0.344
load-independent, load-independent modulus of elasticity, yield 600 1C 0.0147  0.05 0.400 0.374–0.377
700 1C 0.0153  0.07 0.434 0.393–0.399
strength and fracture toughness with Eqs. (2)–(4) are calculated 800 1C 0.0158  0.03 0.462 0.447–0.451
and given in Table 5. Compared to values depending on the load,
load-independent Eo, Yo and KIC values increased. Fracture toughness
is one of the main mechanical properties of the materials. The 3.2.4. Hays–Kendall approach
selection of the materials used for the technological applications is Hays–Kendall concluded that a minimum load is required to
an important parameter. Elastic recovery is not observed in the create a permanent deformation at the sample should be. If this
materials showing the RISE behavior. This case results in an increase resistance does not exceed with the load applied plastic deforma-
in hardness too. In the light of all the results it can be said that the tion does not occur, only elastic. So, Hays and Kendall propose that
obtained results are consistent with the literature [17]. the size of trace experimentally measured is proportional to the
effective load instead of the test load F [20]:
3.2.3. Elastic/Plastic Deformation model 2
F  W HK ¼ AHK d ð10Þ
According to Bull et al. [18,19], dependence of the indentation
size to the applied load for the Elastic/Plastic Deformation model is Here AHK is a constant independent of the load applied. W and AHK
given below values are calculated from the graph F  d2. In this model, load-
independent hardness values are as follows:
F ¼ A2 ðdp þde Þ2 ð8Þ
H HK ¼ 1854:4AHK ð11Þ
Here A2 is a constant and dp is related to the plastic deformation.
A2 and de values can be calculated from F1/2  dp graph (Fig. 8). Therefore, the slope obtained from the graph in Fig. 9 gives the
In this model, the load-independent hardness value is AHK value. Hardness load-independent, WHK and AHK values are
given in Table 7. Negative WHK is the case that is observed in
H EPD ¼ 1854:4A2 ð9Þ
the samples showing the RISE behavior. So, this result can be
In this model, de values in the point where the graph intercepts interpreted as the applied load is only sufficient for the plastic
the y-axis are negative since all the materials show the RISE deformation. When HK model has been analyzed it is seen that the
behavior (Table 6). That is, any elastic deformation could not be results are outside the plateau region. This means that this model
observed in the applied loads. Again, the hardness values calcu- is also insufficient.
lated with this model were quite far from values in the plateau In the models used up to now could not reach hardness values
region. As a result, the EPD model has been insufficient for the around the plateau region for all the samples showing the RISE
hardness analysis of these materials. behavior. For this reason, in addition to these models, IIC model
 M. Tosun et al. / Materials Science & Engineering A 590 (2014) 416–422 421

be calculated for the doped samples

!m
F 5=3
Hv ¼ K 3
ð13Þ
d

Values of K and m are constants independent of the load and is

obtained from the ln (Hv)  ln (F5/3/d3) graph (Fig. 10). Superscript
m is used to explain the ISE or the RISE behaviors. When m 40.6
the material shows a normal ISE behavior, however when m o0.6
the material shows RISE behavior [19,22].
This model gives the most suitable result for the materials
showing the RISE behavior since elastic deformation is not
observed in all samples for the hardness analysis. In Table 8, the
index m obtained from the slope of the graph 0.291, 0.282, 0.298
and 0.290 were found for the samples annealed at 500, 600, 700
and 800 1C respectively. As mentioned above, when m 40.6 the
material shows the normal ISE behavior, but when m o0.6 it
shows the RISE behavior. Looking at the m values obtained from
Fig. 10 it is clear that all samples show the RISE behavior.
In the end, all results are summarized in Table 9.

Fig. 9. Applied load versus the square of the impression semi-diagonal length for
the samples.

Table 7
Best-fit results of experimental data according to HK model.

Samples AHK (GPa) WHK (N) HHK (GPa) Hv (GPa)

4
500 1C 1.88  10   0.058 0.348 0.340–0.344
600 1C 2.06  10  4  0.051 0.382 0.374–0.377
700 1C 2.19  10  4  0.065 0.406 0.393–0.399
800 1C 2.44  10  4  0.028 0.452 0.447–0.451

which has been developed to explain the RISE behavior is used for
microhardness analyses for all samples.

3.2.5. Indentation-Induced Cracking (IIC) model

This model is developed to describe the reverse ISE behavior by
Li and Bradt [21]. According to the model, the applied test load is
balanced in the maximum depth by the total sample resistance.
According to Li and Bradt, friction (slip) and elastic effects lead to Fig. 10. Variation of ln Hv with ln(F5/3/d3) according to IIC model for all samples.

the normal ISE behavior, notch slits (indentation cracking) will

cause the RISE behavior in the material. Li and Bradt stated the
Table 8
importance of the elastic and frictional effects in the PSR model Best-fit results of experimental data according to IIC model.
too. In this model, calculated value of Vickers hardness by the
diamond indenter is given as Samples m K  104 (N(3  5m)/3/mm(2  3m)) HIIC (GPa) Hv (GPa)

 ! 500 1C 0.291 0.0014 0.318 0.340–0.344

F F 5=3 600 1C 0.282 0.0013 0.347 0.374–0.377
H v ¼ λ1 K 1 2
þ K2 3
ð12Þ
d d 700 1C 0.298 0.0016 0.354 0.393–0.399
800 1C 0.290 0.0015 0.394 0.447–0.451

Here d is the trace's diameter and λ1, K1 and K2 are constants.

While K2 value is dependent on the load applied K1 on the
geometry of the indenter. Table 9
While Hv ¼K1(F/d2), λ1 ¼ 1 and K2 (F5/3/d3) ¼0 for an ideal plastic The results of load-dependent Vickers microhardness at the plateau region and
materials Hv ¼K2(F5/3/d3) and λ1 ¼0 for ideal brittle solids. d ¼7h load-independent hardness values calculated using PSR, MPSR, EPD and HK models
for Eq. (12). This equation is related to an angle of 1481 between
Samples Hv (GPa) (in plateau HPSR HEPD HHK HIIC
the opposing edges of the indenter, h is the depth of the region) (GPa) (GPa) (GPa) (GPa)
indentation. If the investigated material is a brittle material only
second part of the equation is used as will be stated below. In this 500 1C 0.340–0.344 0.370 0.373 0.348 0.318
study, the elastic deformation was not observed in the doped 600 1C 0.374–0.377 0.402 0.400 0.382 0.347
700 1C 0.393–0.399 0.430 0.434 0.406 0.354
samples. Therefore, they have greater brittleness. So, Eq. (13) 800 1C 0.447–0.451 0.463 0.462 0.452 0.394
derived from Eq. (12) is analyzed, the best hardness results can
422 M. Tosun et al. / Materials Science & Engineering A 590 (2014) 416–422

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Acknowledgments

This research was supported by Bahcesehir University

Research Fund.