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Arabian Journal of Chemistry (2015) xxx, xxx–xxx
King Saud University
Arabian Journal of Chemistry
www.ksu.edu.sawww.sciencedirect.com
REVIEW
Conductivity study by complex impedance
spectroscopy of Na3Nb4As3O19
* Corresponding author at: Laboratoire de Materiaux et
Cristallochimie, Faculte des Sciences de Tunis, Universite de Tunis
El Manar, 2092 El Manar II, Tunis, Tunisia.
E-mail address: [email protected] (S.F. Cherif).
Peer review under responsibility of King Saud University.
Production and hosting by Elsevier
http://dx.doi.org/10.1016/j.arabjc.2015.09.0011878-5352 � 2015 The Authors. Production and hosting by Elsevier B.V. on behalf of King Saud University.This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Please cite this article in press as: Cherif, S.F. et al., Conductivity study by complex impedance spectroscopy of Na3Nb4As3O193Nb4As3O19 –>. Arabian JoChemistry (2015), http://dx.doi.org/10.1016/j.arabjc.2015.09.001
Saıda Fatma Cherif a,b,*, Mohamed Faouzi Zid a, Ahmed Driss a
aLaboratoire de Materiaux et Cristallochimie, Faculte des Sciences de Tunis, Universite de Tunis El Manar, 2092 El Manar II,Tunis, Tunisiab Institut Preparatoire aux Etudes d’Ingenieurs – El Manar, Universite de Tunis El Manar, 2092 El Manar II, Tunis, Tunisia
Received 7 October 2014; accepted 7 September 2015
KEYWORDS
Three-dimensional frame-
work;
IR spectroscopy;
CI spectroscopy;
Ionic conductivity
Abstract Crystals of Na3Nb4As3O19 were synthesized by a solid-state reaction. It crystallizes in the
orthorhombic system, space group C2221 with a= 13.014(2) A, b= 24.170(3) A and c = 5.0880
(9) A. The structure can be described as a three-dimensional anionic framework containing two
kinds of tunnels parallel to [001] direction where Na+ cations are located. The ionic conductivity
was measured, on pellets of polycrystalline powders, between 573 and 893 K in the frequency range
0.01–13000 kHz through the complex impedance method. A correlation between electrical and
structural properties was also discussed.� 2015 The Authors. Production and hosting by Elsevier B.V. on behalf of King Saud University. This is an
open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2. Experimental section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 002.1. Polycrystalline powder synthesis of Na3Nb4As3O19 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 002.2. Infrared spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
2.3. Ionic conductivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 003. Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.1. Crystal structure and refinement. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
urnal of
2 S.F. Cherif et al.
3.2. Description of the structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
3.3. Infrared spectroscopy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 003.4. Ionic conductivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 003.5. Correlation between electrical and structural properties of Na3Nb4As3O19 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
4. Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00Acknowledgment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00References. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 00
1. Introduction
The synthesis of compounds that contain monovalent cationsand those with tunnel or layer structures is of potential interestdue to their remarkable ionic conductivity (Daidouh et al.,
1999, 1997; Masquelier et al., 1995; Marzouki et al., 2014;Hajji and Zid, 2012; Frigui et al., 2010, 2011). In order to syn-thesize compounds of this type, we have investigated A–Nb–
As–O system (A = monovalent ion). In a previous work, wehave isolated a few novel mixed oxides (Cherif et al., 2011a,b, 2012a,b). Among these compounds, there are those which
exhibit a tunnel structure. Other cases such as K8Nb7As7O39
exhibit a layer structure where potassium cations are locatedin interlayer space (Cherif et al., 2012b).
The purpose of the present paper is to investigate the elec-
trical properties of Na3Nb4As3O19 and to establish correlationbetween its structure and physical properties.
2. Experimental section
2.1. Polycrystalline powder synthesis of Na3Nb4As3O19
All chemicals were commercially available andwere usedwithoutanypurification.A polycrystalline powder ofNa3Nb4As3O19was
synthesized by a solid-state reaction method from a stoichiomet-ric mixture of Na2CO3, As2O5 and Nb2O5. Starting materialswere mixed and ground together in an agate mortar and heated
progressively to 800 �C in porcelain crucible with intermittentcooling and re-grindings.
The powder was analyzed by X-ray powder diffraction,
using a PAN-analytical X’Pert PRO X-ray diffractometerequipped with copper anticathode (kKa = 1.5406 A). The unitcell parameters were refined using Celref 3.0 program(Altermatt and Brown, 1987) and calculated to be as:
a= 13.015(2) A, b = 24.175(4) A and c= 5.0857(1) A. The
Figure 1 Calculated and experimental powder X-ray diffraction
patterns of Na3Nb4As3O19.
Please cite this article in press as: Cherif, S.F. et al., Conductivity study by complexChemistry (2015), http://dx.doi.org/10.1016/j.arabjc.2015.09.001
powder X-ray diffraction pattern was in agreement with
single-crystal structure (Cherif et al., 2012a) (Fig. 1).
2.2. Infrared spectroscopy
The infrared spectrum of Na3Nb4As3O19 was carried out on aPerkin–Elmer FTIR Paragon 1000 PC spectrometer. Thesample was mixed with dried KBr.
2.3. Ionic conductivity
The electrical properties of the title compound have beeninvestigated on a polycrystalline sample using complex
impedance spectroscopy (CIS).Measurements were carried out in a Hewlett-Packard
4192-A automatic bridge monitored by a HP microcomputer.
The frequency/temperature ranges are 0.01–13,000 kHz/300–620 �C, respectively. Pellet of 13 mm diameter and1.66 mm thickness was prepared by pressing the powder
sample at 12 tones. Then the pellets were heated at 500 �Cfor 12 h in order to improve continuity between the grains.Silver electrodes were painted in the two faces of the pellets
with a silver paste to ensure good electrical contact.Correlation between the sample electrical behavior and its
microstructure is also discussed.
3. Results and discussion
3.1. Crystal structure and refinement
A suitable colorless single crystal with (0.35 � 0.25 � 0.16)mm3 dimensions was selected for the structure determination
and refinement. The data were collected on an Enraf-NoniusCAD-4 automatic four-circle diffractometer using Mo Karadiation (k= 0.71073 A) at room temperature. The unit-cell
Table 1 Parameters and final reliability factors of crystal
structure of the Na3Nb4As3O19 compound.
Crystal system Orthorhombic
Space group C2221Cell parameters a = 13.014(2) A
b = 24.170(3) A
c = 5.0880(9) A
Reflections collected 2166
Independent reflections 1757
Rint 0.041
R(F) 0.029
xR(F2) 0.076
impedance spectroscopy of Na3Nb4As3O193Nb4As3O19 –>. Arabian Journal of
Figure 2 Representation of: (a) infinite chains [Nb12O10]1 and (b) infinite ribbons [Nb4O18]1 in Na3Nb4As3O19.
Figure 3 Representation of the junction between chains and
ribbons in Na3Nb4As3O19.
Figure 4 Projection of the structure of Na3Nb4As3O19 along c
axis showing tunnels where Na+ cations are located.
1200 1000 800 600 4000,6
0,7
0,8
0,9
1,0
657
Tran
smitt
ance
(%)
Wave number (cm-1)
424
482
536
761856908
991 514
Figure 5 IR spectrum of Na3Nb4As3O19.
Conductivity study of Na3Nb4As3O19 3
parameters were determined and refined using a least-squaresmethod based upon 25 reflections in the range 10–15�. Theexperimental values, the final structure refinements and theconditions of intensities collection are detailed in previouswork (Cherif et al., 2012a,b).
The essential structural data are shown in Table 1.
Please cite this article in press as: Cherif, S.F. et al., Conductivity study by complexChemistry (2015), http://dx.doi.org/10.1016/j.arabjc.2015.09.001
3.2. Description of the structure
The structure of Na3Nb4As3O19 can be described from NbO6
octahedra and AsO4 tetrahedron sharing vertices. In the anio-nic framework, Nb1O6 octahedra form by sharing vertices infi-
nite chains [Nb12O10]1 running along [001] (Fig. 2a). Nb2O6
and Nb3O6 octahedra are connected by vertices to form infiniteribbons [Nb4O18]1 (Fig. 2b). The junction of these ribbons
and chains is assured by vertices via AsO4 tetrahedron(Fig. 3). It results in a three-dimensional framework withtwo kinds of tunnels parallel to the [001] direction whereNa+ cations are located (Fig. 4).
3.3. Infrared spectroscopy
To investigate the coordination environment of Na3Nb4As3-
O19, the infrared spectroscopy was carried out in the range1200–300 cm�1 and the obtained spectrum is shown in Fig. 5.
The assignment of the different vibrational bands of NbO6
and AsO4 groups based on those found in the literature (BenAmor et al., 2008; Nakamoto, 1978; Bouzemi Friaa et al.,2003; Ouerfelli et al., 2007a,b), is shown in Table 2.
3.4. Ionic conductivity
Fig. 6 shows the complex impedance spectra, Nyquist plots,reflecting the variation of the imaginary part of the complex
impedance spectroscopy of Na3Nb4As3O193Nb4As3O19 –>. Arabian Journal of
Table 2 Assignment of vibration fre-
quencies in Na3Nb4As3O19.
Wave number (cm�1) Assignment
424 m4(AsO4)
482 m4(NbO6)
514
536
657 m2(NbO6)
761 m3(NbO6)
856 m1(AsO4)
908 m3(AsO4)
991
Figure 7 (a) The ln(rT) versus 104/T plot. (b) The ln(fmax) versus
104/T plot, where fmax is the Z00max peak frequency.
4 S.F. Cherif et al.
impedance (�Z00) versus its real part (Z0) at various tempera-tures and a wide range of frequency. The impedance spectra
are characterized by the appearance of a single semicirculararc with their centers below the real axis. The measuredimpedance can be modeled as equivalent electrical circuits
comprising of a parallel combination of bulk resistance andCPE; which is the non-ideal capacitor usually known asconstant phase element (Anantha and Hariharan, 2005).
For each temperature, we determine the value of Z byZView program (ZView Version 3.1c, 1990–1997). The ionicconductivity as function of the temperature has been obtainedfrom the values of intercept of the extrapolated high-frequency
semicircles with the real axis. As a consequence, the value ofthe conductivity r governed by the relationship (1) is calcu-lated as follows:
0 20000 40000 60000 800000
10000
20000
30000
40000
460°C 440°C420°C-Z
'' (o
hm)
Z' (ohm)
Z' (ohm)0 1000 2000 3000 4000 5000
0
500
1000
1500
2000
2500
580°C 560°C 540°C-Z''
(ohm
)
0 60000 120000 1800000
30000
60000
90000
340°C320°C
300°C
-Z''
(ohm
)
Z' (ohm)
Figure 6 Complex impedance spectrum of Na3Nb4
Please cite this article in press as: Cherif, S.F. et al., Conductivity study by complexChemistry (2015), http://dx.doi.org/10.1016/j.arabjc.2015.09.001
r ¼ ðe=sÞ=Z ðX�1 cm�1Þ ð1ÞThe conductivity variation indicates an increase in conduc-
tivity with rise in temperature with a typical Arrhenius-typebehavior: linear dependence of thermal conductivity logarithmln(rT) versus 104/T (K�1) (Fig. 7a). This type of temperature
dependence of the conductivity indicates that the electricalconduction in the materials is a thermally activated process.It can be explained in accordance with the expression (2) as
follows:
0 40000 80000 1200000
20000
40000
60000
400°C380°C
360°C-Z''
(ohm
)
Z' (ohm)
0 5000 10000 15000 200000
2500
5000
7500
10000
520°C 500°C480°C-Z
'' (o
hm)
Z' (ohm)
0 500 1000 1500 20000
250
500
750
1000
620°C610°C
600°C
-Z''
(ohm
)
Z' (ohm)
As3O19 over temperature range 300 and 620 �C.
impedance spectroscopy of Na3Nb4As3O193Nb4As3O19 –>. Arabian Journal of
Figure 8 Variation of imaginary part of impedance (�Z00) with frequency at various temperatures.
Figure 9 A zoom of the differential scanning calorimetry curve
of Na3Nb4As3O19.
Figure 10 Dimensions of the large tunnel in Na3Nb4As3O19
structure.
Figure 11 Dimensions of the hexagonal tunnel in Na3Nb4As3-
O19 structure.
Conductivity study of Na3Nb4As3O19 5
Please cite this article in press as: Cherif, S.F. et al., Conductivity study by complexChemistry (2015), http://dx.doi.org/10.1016/j.arabjc.2015.09.001
rT ¼ A0 expð�Ea=kTÞ ð2Þ
where A0 is the pre-exponential factor, Ea is the activationenergy, T is the absolute temperature and k is the Boltzmannconstant.
impedance spectroscopy of Na3Nb4As3O193Nb4As3O19 –>. Arabian Journal of
Table 3 Occupancies of Na+ cations.
Atoms x y z Occupancies Wyckoff
Na1 0.2677(4) 1/2 0 0.937(16) 4a
Na2 0.0494(12) 1/2 1/2 0.68(3) 4a
Na3 0.184(4) 1/2 1/2 0.092(18) 4a
Na4 0.105(7) 1/2 1/2 0.11(3) 4a
Na5 0.771(3) 0.7465(10) 0.753(13) 0.12(2) 8c
Na6 0.742(4) 0.7414(15) 0.629(18) 0.11(3) 8c
Na7 0.7659(13) 0.7594(7) 0.006(11) 0.191(16) 8c
Na8 0.7726(19) 0.7525(11) 0.892(12) 0.17(2) 8c
6 S.F. Cherif et al.
Fig. 8 shows the variation of the imaginary part of impe-dance with frequency (loss spectra) at different temperatures.
The spectra are characterized by the presence of peaks at aparticular frequency. As temperature increases the magnitudeof Z00 peak maxima decreases and the peak frequency shifts
to higher values. These results suggest the presence of electricalrelaxation in the material, which depends on temperature(Kumer and Manna, 2008). The variation of peak frequency,
fmax as function of temperature which obeys to Arrheniusrelation (3) is shown in Fig. 7b.
fmax ¼ f0 expð�Ef=kTÞ ð3ÞThe activation energy corresponding to electrical relaxation
has been calculated to be Ea(1) = 0.98 eV at high temperaturesand Ea(2) = 0.35 eV at low temperatures, which is almost
equal to those found from relation (2): Ea(1) = 0.94 eV andEa(2) = 0.39 eV.
3.5. Correlation between electrical and structural properties ofNa3Nb4As3O19
At 440 �C, we observe the change of the slope in the plot of ln(rT) against reciprocal temperature (Fig. 6a) which is due to
Table 4 Conductivity r (X�1 cm�1) and conduction activation ener
Compound Temperature range (K) Ea (e
Low ionic conductors
Na3Nb4As3O19 573–713 0.39
KFeAs2O7 558–668 0.47
Mild ionic conductors
NaCa1.5(NbO)2O2(AsO4)2 900–963 2.15
K3Cr3(AsO4)4 563–703 1.21
Ag0.62K0.38Nb4AsO13 603–883 0.807
Ag4Co7(AsO4)6 403–483 0.45
NaCa1.5(NbO)2O2(AsO4)2 703–900 1.14
Na0.5K0.65Mn3.43(AsO4)3 493–673 0.762
KMn6(As2O7)2(As3O10) 663–843 1.11
Good ionic conductors
Ag12.4Na1.6Mo18As4O71 448–693 0.763
TlFe0.22Al0.78As2O7 623–808 0.656
Li3Sc2(AsO4)3 400–600 0.910
Na3Nb4As3O19 713–893 0.94
Very good ionic conductors
Li3Fe2(AsO4)3 400–600 0.710
Na3Sc2(AsO4)3 400–600 0.460
Please cite this article in press as: Cherif, S.F. et al., Conductivity study by complexChemistry (2015), http://dx.doi.org/10.1016/j.arabjc.2015.09.001
transition phase or the existence of two mechanisms of ionicconductivity. To distinguish between these two possibilities,
Differential Scanning Calorimetry (DSC) analysis of Na3Nb4-As3O19 has been conducted over the temperature range 25–485 �C. A zoom of the thermal analysis results in the range
400–485 �C is shown in Fig. 9.At 440 �C, DSC thermogram does not present any phase
transition or other thermal phenomenon. This result con-
firms the existence of two mechanisms of ionic conductivitygoverned by the crystallographic structure.
In fact, according to the data of the structural study of Na3-Nb4As3O19, there are two kinds of tunnels where Na+ cations
are located. Their section dimensions are illustrated in Figs. 10and 11.
The first type of tunnels is large (Fig. 10) with maximum
cross equal to 13.014 A containing a bottleneck of smallwidth equal to 4.705 A which is inferior to 2(rO2- + rNa+) =2(1.38 + 1.12) = 5 A according to Shannon (1976).
However, the second type of tunnels (Fig. 11) has hexago-nal section. The dimensions of these tunnels vary from 6.354 to9.390 A. Both of them are longer than twice the sum of rayrO2- = 1.38 A and rNa+ = 1.02 A according to Shannon
(1976).
gy Ea (eV) of previous works.
V) r (X�1 cm�1) Reference
r733K = 2.68 � 10�6
This work
r668K = 0.28 � 10�6 Ouerfelli et al. (2007a,b)
r963K = 9.73 � 10�5 Ben Amor et al. (2008)
r703K = 4.61 � 10�5 Bouzemi Friaa et al. (2003)
r883K = 3.87 � 10�5 Cherif et al. (2011)
r483K = 3.3 � 10�5 Marzouki et al. (2014)
r900K = 1.13 � 10�5 Ben Amor et al. (2008)
r673K = 0.89 � 10�5 Frigui et al. (2011)
r843K = 0.65 � 10�5 Frigui et al. (2010)
r713K = 4.66 � 10�4 Hajji and Zid (2012)
r808K = 3.45 � 10�4 Ouerfelli et al. (2007a,b)
r600K = 1.40 � 10�3 Goodenoough et al. (1976)
r893K = 1.15 � 10�4
This work
r600K = 7.60 � 10�3 Goodenoough et al. (1976)
r600K = 1.70 � 10�3 Goodenoough et al. (1976)
impedance spectroscopy of Na3Nb4As3O193Nb4As3O19 –>. Arabian Journal of
Conductivity study of Na3Nb4As3O19 7
Adding to this, the presence of Na+ cations with a partialoccupancy facilitates their mobility. We report in Table 3 theoccupancies of these cations.
These geometric factors are causing an ion mobility reach-ing 1.15 � 10�4 X�1 cm�1 at 893 K and 2.68 � 10�6 X�1 cm�1
at 733 K. These values, compared to those found in other com-
pounds, enable us to conclude that our compound can beplaced in the family of low ionic conductors at lowtemperatures and the family of good ionic conductors at high
temperatures (Table 4).
4. Conclusion
Crystals of Na3Nb4As3O19 were obtained by a solid-statereaction. Different characterization techniques have been used:infrared spectroscopy, powder X-ray diffraction and ionic
conductivity. The structure of this material has an open frame-work delimiting two kinds of tunnels parallel to [001] whereNa+ cations are located. Ionic conductivity study versustemperature is undertaken. It reveals that this material can
be classified as low ionic conductor at low temperatures andas good ionic conductor at high temperatures.
Acknowledgment
The authors gratefully acknowledge the financial support
of Ministry of Higher Education, Scientific Research andTechnology of Tunisia.
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