Microstructure and piezoelectric properties of (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 ceramics

Hitoshi Nishijima; Tasuku Kawashima; Ryosuke S.S. Maki; Yoshikazu Suzuki

doi:10.1016/j.arabjc.2016.12.017

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Original article

12 (

); 5253-5259

doi:

10.1016/j.arabjc.2016.12.017

Microstructure and piezoelectric properties of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ ceramics

Hitoshi Nishijima^{^a}, Tasuku Kawashima^{^a}, Ryosuke S.S. Maki^{^a}, Yoshikazu Suzuki^{^a,^b,⁎}

a Graduate School of Pure and Applied Sciences, University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8573, Japan

b Faculty of Pure and Applied Sciences, University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8573, Japan

⁎Corresponding author at: Faculty of Pure and Applied Sciences, University of Tsukuba, Ibaraki 305-8573, Japan. suzuki@ims.tsukuba.ac.jp (Yoshikazu Suzuki)

Received: 2016-6-28, Accepted: 2016-12-24, Published: 2016-12-01

Disclaimer:
This article was originally published by Elsevier and was migrated to Scientific Scholar after the change of Publisher.

Peer review under responsibility of King Saud University.

Abstract

In this paper, we report the synthesis, microstructure and some piezoelectric properties of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ (abbreviated as BNBTFN, x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100). The BNBTFN powders were prepared by solid-state reaction method, and their green compacts were sintered at 1150 °C for 2 h. XRD study confirmed that there was no second phase for all the compositions. Morphotropic phase boundary (MPB) of rhombohedral and tetragonal phases existed at x ∼ 0.050, which was close to that of the BNT-BT system. With increasing x, diffuse phase transition, decrease in transition temperature (T_m), and increase in dielectric maximum at the transition temperature (ε_rm) were observed. The A and B sites simultaneous substitutions, i.e. Ba²⁺ into (Bi_0.5Na_0.5)²⁺ and (Fe_0.5Nb_0.5)⁴⁺ into Ti⁴⁺, have some positive effects on piezoelectric properties for x ⩽ 0.05 of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃, despite the lowering of depolarization temperature.

Keywords

Lead-free piezoelectric ceramics

Dielectric properties

BNT-BT

Solid-state reaction

Morphotropic phase boundary (MPB)

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1 Introduction

Piezoelectric ceramics are widely used in electric devices such as actuators, sensors, transducers and so on. Lead zirconate titanate (PZT) based ceramics are prevailing in piezoelectric devices due to their superior piezoelectric properties (Jaffe et al., 1955; Damjanovic, 1998; Noheda, 2002 ). However, PZT-based ceramics contain highly-concentrated lead which is considered as a harmful substance (Maeder et al., 2004). Lead-free piezoelectric ceramics replacing PZT are strongly required (Takenaka et al., 2007; Panda, 2009; Rödel et al., 2009; Aksel and Jones, 2010 ). (K, Na)NbO₃ (KNN)-based and Bi_0.5Na_0.5TiO₃ (BNT)-based systems have been extensively studied as candidate lead-free systems.

For the KNN-based system, high piezoelectric constant d₃₃ of ∼400 pC/N have been reported (Rubio-Marcos et al., 2007, 2015; Bortolani et al., 2014 ). Meanwhile, BNT with perovskite (ABO₃) structure has been considered as another promising candidate (Smolenskii and Agranovskaya, 1960). BNT shows excellent piezoelectric properties, e.g. remnant polarization P_r = 38 μC/cm², and the Curie temperature T_c = 320 °C. However, BNT is hard to be poled due to its large coercive field E_C = 73 kV/cm (Takenaka et al., 1991), which restricts device applications. To overcome such restrictions, various BNT-based perovskite-type solid solutions particularly near the morphotropic phase boundary (MPB) have been developed, such as Bi_0.5Na_0.5TiO₃-BaTiO₃ (BNT-BT) (Takenaka et al., 1991; Maurya et al., 2013), Bi_0.5Na_0.5TiO₃-Bi_0.5K_0.5TiO₃ (BNT-BKT) (Nagata et al., 2003; Li and Tan, 2016), Bi_0.5Na_0.5TiO₃-K_0.5Na_0.5NbO₃ (BNT-KNN) (Hao et al., 2012), and Bi_0.5Na_0.5TiO₃-Bi_0.5K_0.5TiO₃-BaTiO₃ (BNT-BKT-BT) (Wang et al., 2004; Maurya et al., 2015).

To date, both the A-site substitution (Herabut and Safari, 1997; Cheng et al., 2013; Qu et al., 2005 ) and the B-site substitution (Yu et al., 2007; Danwittayakul et al., 2008; Davies et al., 2011 ) have been widely investigated. As for the B-site substitution, for example, Zhou et al. reported that co-substitutions to Ti⁴⁺ by (Ni_1/3Nb_2/3)⁴⁺ (Zhou and Liu, 2008a), (Mg_1/3Nb_2/3)⁴⁺ (Zhou et al., 2009) and (Zn_1/3Nb_2/3)⁴⁺ (Zhou and Liu, 2008b) were effective to improve piezoelectric coefficient d₃₃.

Co-substitutions to Ti⁴⁺ by (Fe_0.5Nb_0.5)⁴⁺ are also a promising strategy (Suzuki and Abe, 2014). Amouri et al. (2014) have recently reported a new system, (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ (x = 0, 0.025, 0.05, 0.075 and 0.1). In their report, although a diffuse phase transition and better dielectric permittivity were observed, the piezoelectric properties were not reported. In this paper, we report the microstructure and some piezoelectric properties of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100), hereinafter BNBTFN.

2 Experimental procedure

BNBTFN powders were prepared by solid-state reaction method. Bi₂O₃ (99.9% purity, Wako Pure Chemical Industries Ltd., Osaka, Japan), anhydrous Na₂CO₃ (99.8%, Wako), BaCO₃ (99.9%, Wako), TiO₂ (anatase) (99.9%, Kojundo Chemical Laboratory Co. Ltd, Saitama, Japan), α-Fe₂O₃ (99.9% purity, Wako) and Nb₂O₅ (99.9% purity, Wako) were used as starting materials for (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100). The stoichiometric amounts of the starting powders were wet-ball milled in ethanol using zirconia balls as grinding media for 24 h. The mixed slurries were dried, and then sieved through <100 μm mesh screen. The mixed powders in an alumina crucible were heated at 200 °C for 2 h to remove adsorbed water, and then, were calcined at 850 °C for 2 h (heating rate: 100 °C/h). The calcined powders were wet-ball milled in ethanol for 2 h, dried and sieved (<100 μm) to obtain the BNBTFN powders. Then, the powders were mixed with some 2.5 wt% poly(vinyl alcohol) aq. as a binder. The powders were pressed into green compacts by uniaxially mold pressing at 16.6 MPa for 1 min. Then, the green compacts (diameter: ca. 10 mm) were pressed by cold isostatic pressing (CIP) at 200 MPa for 10 min. The pellets in a covered alumina crucible were first degreased at 500 °C for 2 h, and then sintered at 1150 °C for 2 h (heating rate: 100 °C/h). To minimize the evaporation of volatile elements (i.e. Bi and Na), the samples were embedded in the powders with the same composition. The sintered samples were polished by waterproof abrasive papers (#1200). The final thickness of the samples was ∼1.5 mm. In order to measure dielectric and piezoelectric properties, silver paste as an electrode was formed on both sides of the polished samples by firing at 700 °C for 100 min. The samples for piezoelectric measurements were poled in silicone oil bath under ∼4 kV/mm for 10 min at room temperature to 80 °C. The samples for the grain-size measurement were mirror-polished using 9.0, 3.0 and 0.5 μm sized diamond slurries. The mirror polished samples were thermally etched at 950 °C for 2 h (heating rate: 200 °C/h).

The constituent phases of the samples were analyzed by X-ray diffraction (XRD, Multiflex, Cu-Kα, 40 kV and 40 mA, Rigaku, Tokyo, Japan). Rietveld refinement of the XRD patterns was carried out by using RIETAN-FP software (Izumi and Momma, 2007). The surface morphology of the mirror-polished samples was characterized by using scanning electron microscopy (SEM; JSM-5600/SV, JEOL, Tokyo, Japan). The chemical composition on the bulk samples was measured by scanning electron microscopy (Hitachi TM3000, operated at 15 kV) equipped with energy dispersive X-ray spectrometry (SEM–EDS). The bulk density of sintered pellets was calculated from dimension and mass. The temperature dependences of dielectric constant (ε_r) and tangent loss (tanδ) were measured using an impedance analyzer (Agilent HP4192A, Santa Clara, CA) at 10 kHz in the temperature range of 30–400 °C. The planar electromechanical coupling coefficient k_p was determined by a resonance (f_r)-antiresonance (f_a) method through the impedance spectrum. The piezoelectric constant d₃₃ was measured using a quasi-static d₃₃ meter (ZJ-6B, IACAS, Beijing, China) after aging for at least 24 h from the poling process. The average grain size of thermal-etched samples was determined by an image analysis (Image J software) for ca. 400–600 grains in SEM images.

3 Results and discussion

3.1

3.1 Constituent phases and microstructure

Fig. 1a shows XRD patterns of BNBTFN sintered samples. There was no second phase formation for all the compositions. In accordance with the report of Amouri et al. (2014), systematic peak shifts to lower angles with increasing x were observed, i.e. by the co-substitution of Ba²⁺ into (Bi_0.5Na_0.5)²⁺ and (Fe_0.5Nb_0.5)⁴⁺ into Ti⁴⁺. The peak shifts mean the increase in unit cell size by the substitution of larger ions; Shannon's effective ionic radii (r) of the A-site cations (12 coordination) are r(Ba²⁺) = 1.61 Å, “r(Bi³⁺) ∼ 1.38 Å” and r(Na⁺) = 1.39 Å, and those of the B-site cations (6 coordination) are r(Fe³⁺) = 0.645 Å, r(Nb⁵⁺) = 0.64 Å and r(Ti⁴⁺) = 0.605 Å (Shannon, 1976). Note that the ionic radius for 12-coordination Bi³⁺ was not listed in the Shannon's table, but can be estimated as r(Bi³⁺) ∼ 1.38 Å from the extrapolation of Shannon's data for 5, 6 and 8 coordinations. This estimation seems to be reasonable because the 8-coordination r(Na⁺) = 1.18 Å and r(Bi³⁺) = 1.17 Å are listed in the table. Eitel et al. (2001) used r(Bi³⁺) = 1.34 Å and Suchomel and Davies (2004) used r(Bi³⁺) = 1.36 Å for the 12-coordination Bi³⁺, by using similar extrapolation method but with more nonlinearity.

(a) XRD patterns and (b) estimated lattice volume of (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100). In (b), 6VT is plotted for x = 0.065–0.100.

In the present study, rhombohedral phase (R3c (161), Jones and Thomas, 2002) was observed for x = 0.000, 0.025 and 0.050, and tetragonal phase (Pmmm (99)), or substantially pseudocubic, was observed for x = 0.050, 0.065, 0.075 and 0.100; mixture of rhombohedral and tetragonal phases was observed for x = 0.050. These results are somewhat different from those of the Amouri's report where orthorhombic phase was observed for x = 0.025 and 0.050. The phase difference of intermediate compositions might be attributable to the difference of sintering program, i.e., at 1150 °C for 2 h in this research whereas at 1050–1170 °C (depending on the compositions) for 5 h in the Amouri's report. Note that in the BNT-BT system, Takenaka et al. (1991) reported that the MPB between rhombohedral BNT and tetragonal BT exists near the composition of x = 0.06, i.e., 0.94(Bi_0.5Na_0.5)TiO₃-0.06BaTiO₃. Table 1 summarizes the estimated lattice parameters of rhombohedral and tetragonal phases in this study. Lattice volume in Table 1 is plotted in Fig. 1b, which clearly shows the monotonical lattice expansion with increasing x.

Table 1 Lattice parameters of rhombohedral (R3c) and tetragonal (P4bm) (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ phases in this study.

x	a_H (Å)	c_H (Å)	V_H (Å³)	a_T (Å)	c_T (Å)	V_T (Å³)	6V_T (Å³)
x = 0.000	5.4823(8)	13.519 (1)	351.91(8)
x = 0.025	5.4967(7)	13.541(1)	354.31 (7)
x = 0.050	5.519(2)	13.522(8)	356.8(3)	3.9024(4)	3.9040(9)	59.45(2)	356.7
x = 0.065				3.9070(7)	3.9052(9)	59.61(2)	357.7
x = 0.075				3.9111(5)	3.910(1)	59.81(2)	358.9
x = 0.100				3.916(1)	3.916(2)	60.06(4)	360.4

Hexagonal unit cell is used for the rhombohedral phase.

Fig. 2 shows SEM surface images of BNBTFN sintered samples, and Table 2 summarizes their average grain size obtained from the SEM images. From Fig. 2 and Table 2, it is revealed that the grain size distribution was not so different to each other; the average grain sizes were ∼1.0–1.5 μm (see more detail in Fig. S1). Some elongated grains found in the pictures might be attributed to Na-lean phases such as Na₂Ti₆O₁₃ (not evidently detected in Fig. 1). Ramajo et al. (2015) have studied in detail the effect of such secondary phases on ferroelectric properties of Bi(Na,K)TiO₃ ceramics through confocal Raman spectroscopy.

SEM images of (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100).

Table 2 Average grain size of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃.

Amount x of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x (Fe_0.5 Nb_0.5)_xO₃	Average grain size (μm)	Standard deviation
x = 0.000	1.26	0.63
x = 0.025	1.06	0.49
x = 0.050	1.07	0.47
x = 0.065	1.30	0.58
x = 0.075	1.18	0.52
x = 0.100	1.09	0.53

The relative density values of all samples were estimated to be >95.5% (Fig. S2), which was in good agreement with the SEM observation. Table 3 summarizes the nominal and EDS-measured cationic compositions. Thanks to the powder-bed sintering technique, the deviation between nominal and measured cationic compositions was not so different to each other. As is expected, some Na loss was observed, and hence, the compositions of heavier elements (Ba and Ta) became somewhat increased. Note that EDS analyses for minor elements may contain more errors than major elements due to the background.

Table 3 Nominal and EDS-measured cationic compositions for some selected compositions of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃. Measured values for 4 areas were averaged for each composition.

x		Bi (at.%)	Na (at.%)	Ba (at.%)	Ti (at.%)	Fe (at.%)	Nb (at.%)
x = 0.025	Nominal	24.4	24.4	1.3	48.8	0.6	0.6
x = 0.025	Measured	26.6	23.3	3.0	45.1	0.6	1.4
x = 0.050	Nominal	23.8	23.8	2.5	47.5	1.3	1.3
x = 0.050	Measured	25.9	22.3	4.7	43.9	1.1	2.0
x = 0.075	Nominal	23.1	23.1	3.8	46.3	1.9	1.9
x = 0.075	Measured	24.9	21.1	6.1	42.9	2.1	2.8

3.2

3.2 Dielectric and piezoelectric properties

Fig. 3 shows temperature dependences of (a) dielectric constant and (b) dielectric loss tangent of BNBTFN sintered samples, measured at 30–400 °C. With increasing x, maximum dielectric constant ε_rm became larger, and was the largest at x = 0.050 (Fig. 3a). This result was in good agreement with the XRD results where the MPB existed around x = 0.050.

Temperature dependences of (a) dielectric constant and (b) dielectric loss tangent (at 10 kHz) of (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100).

As for the dielectric loss tangent, tanδ at room temperature became larger with increasing x (Fig. 3b). The peaks of tanδ in Fig. 3b (i.e., the shoulder peaks of ε_r in Fig. 3a), corresponding to the depolarization temperature T_d, shifted to lower temperatures with increasing x; T_d = 189, 145, and 50 °C for x = 0.000, 0.025 and 0.050, respectively. There was no obvious T_d for x = 0.065, 0.075 and 0.100, which indicated that the samples of these compositions can be antiferroelectric (or paraelectric). In fact, for the sample with x = 0.050 (T_d = 50 °C), the poling treatment was impossible at 80 °C and done at 25 °C. For the sample with x ⩾ 0.065, the poling treatment was impossible even at 5 °C. The phase transition temperatures also shifted to lower temperatures with increasing x (Fig. 3a). These results indicated that excess substitution is not favorable for the piezoelectric properties.

The maximum dielectric constant temperature T_m was 330 °C for x = 0.000, whereas it was 250 °C for x = 0.100. The large dielectric constant (Fig. 3a), diffuse phase transition (Fig. 3a and b), and frequency dependence of dielectric constant (Fig. 4) suggest that the BNBTFN ceramics are relaxor ferroelectrics. The diffuseness of relaxors (diffuse coefficient) $γ$ is expressed as the modified Curie–Weiss empirical formula proposed by Uchino and Nomura (1982): $\frac{1}{ε_{r}} - \frac{1}{ε_{rm}} = \frac{{(T - T_{m})}^{γ}}{K}$ where ε_rm is dielectric maximum at the transition temperature T_m, K is a constant, and T is absolute temperature. Fig. 5 shows the [ln(T − T_m)] versus [ln((1/ε_r) − ln(1/ε_rm))] plot for x = 0.000, 0.050 and 0.075, and the diffuse coefficient $γ$ at 10 kHz. $γ$ = 1 means ideal ferroelectrics and $γ$ = 2 means ideal relaxor. With increasing x, $γ$ became close to 2, indicating more diffuse phase transition.

Temperature and frequency dependences of (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 (x = 0.065).

Plots of [ln(T − Tm)] versus [ln((1/εr) − ln(1/εrm))] for (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 (x = 0.000, 0.050 and 0.075).

For BNT-BT, dielectric constant ε_r became larger with increasing BT substitution (i.e., Ba²⁺ substitution into (Bi_0.5Na_0.5)²⁺ (Takenaka et al., 1991; Xu et al., 2008). In contrast, for the BNBTFN in this study, ε_r became smaller for x ⩾ 0.065, because the B-site substitution by (Fe_0.5Nb_0.5) into Ti⁴⁺ tends to decrease the dielectric constant.

Fig. 6 shows piezoelectric properties of BNBTFN ceramics. Piezoelectric constant d₃₃ and planer coupling factor k_p increased with x, and showed maximum values of d₃₃ = 129 pC and k_p = 0.27 for x = 0.050, close to the MPB. On the other hand, for x ⩾ 0.065, d₃₃ was less than 10 pC/N and k_p could not be calculated due to the difficulty of poling treatment. The mechanical quality factor Q_m is estimated to be 155, 137 and 21 for x = 0.000, 0.025 and 0.050, respectively. The piezoelectric coefficients (d₃₃ and kp) of the previously reported BNT-based ceramics are well-reviewed by Villafuerte-Castrejón et al. recently (Villafuerte-Castrejón et al., 2016). The d₃₃ value in this study was comparable to the reported values, but the k_p value was rather small. Further optimization of the sintering conditions, etc. is still needed.

Piezoelectric constant d33 and planer coupling factor kp of (Bi0.5Na0.5)1−xBaxTi1−x(Fe0.5Nb0.5)xO3 (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100).

4 Conclusions

In this study, we reported the microstructure and some dielectric and piezoelectric properties of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ ceramics (x = 0.000, 0.025, 0.050, 0.065, 0.075 and 0.100). With increasing x, diffuse phase transition, decrease in transition temperature (T_m), and increase in dielectric maximum at the transition temperature (ε_rm) were observed. MPB of rhombohedral and tetragonal phases was confirmed around x = 0.050. The A and B-sites simultaneous substitution in this study, i.e. Ba²⁺ into (Bi_0.5Na_0.5)²⁺ and (Fe_0.5Nb_0.5)⁴⁺ into Ti⁴⁺, has some positive effects on piezoelectric properties for x ⩽ 0.05 of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃, despite the lowering of depolarization temperature. As a future work, the temperature and time stabilities of piezoelectric properties should be studied.

Acknowledgment

We really thank the anonymous reviewers to improve our manuscript. Their comments are excellent and so helpful. We also appreciate Prof. T. Koyano at University of Tsukuba for the help of SEM observation.

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Appendix A

Supplementary material

Supplementary data associated with this article can be found, in the online version, at http://dx.doi.org/10.1016/j.arabjc.2016.12.017.

Appendix A

Supplementary material

Supplementary data 1

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Introduction

Experimental procedure

Results and discussion

Constituent phases and microstructure
Dielectric and piezoelectric properties

Conclusions

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[Google Scholar]

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Microstructure and piezoelectric properties of (Bi_0.5Na_0.5)₁₋_xBa_xTi₁₋_x(Fe_0.5Nb_0.5)_xO₃ ceramics

Abstract

Keywords

Lead-free piezoelectric ceramics

Dielectric properties

BNT-BT

Solid-state reaction

Morphotropic phase boundary (MPB)

1 Introduction

2 Experimental procedure

3 Results and discussion

3.1 Constituent phases and microstructure

3.2 Dielectric and piezoelectric properties

4 Conclusions

Acknowledgment

References

Appendix A

Supplementary material

Appendix A

Supplementary material

Supplementary data 1

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