The (1-x)BiFeO3-xBaTiO3-Bi(Zn0.5Ti0.5)O3 high temperature lead-free piezoelectric ceramics with strong piezoelectric properties

doi:10.21203/rs.3.rs-329232/v1

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The (1-x)BiFeO3-xBaTiO3-Bi(Zn0.5Ti0.5)O3 high temperature lead-free piezoelectric ceramics with strong piezoelectric properties

https://doi.org/10.21203/rs.3.rs-329232/v1

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published 11 Jul, 2021

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The structure, microstructure, piezoelectric properties, ferroelectric properties and Curie temperature of (1- x )BiFeO 3 - x BaTiO 3 -Bi(Zn 0.5 Ti 0.5 )O 3 +MnO 2 +Li 2 CO 3 ceramics were investigated experimentally by improved solid-state reaction approach. The crystalline structures were examined by X-ray diffractometry. When x = 0.3, the rhombohedral and pseudocubic phases coexist in the ceramic structure. It is considered that the morphotropic phase boundary was formed here. At the same time, the piezoelectric performance d 33 , Curie temperature T C , and depolarization temperature are as high as 184 pC/N, 550°C, 530°C at x = 0.3, respectively. It is worth noting that when x = 0.24, the ceramics have a high T C = 580°C and low dielectric loss tan δ = 1.9%. These results show that the BFBT-BZT system ceramics are applicable ceramics with high piezoelectric properties in high temperature fields.

Electronic Materials and Devices

Ceramics

BiFeO3-BaTiO3

Piezoelectric

Lead-free piezoelectric ceramics

Phase structure

High Curie temperature

Piezoelectric ceramics are commonly used in sensors, transducers and many other fields [1,2,3]. High temperature piezoelectric materials may be applied in nuclear energy, oil well drilling, aerospace vehicles, geological mining [4,5]. PZT ceramics are a kind of piezoelectric ceramic material which are widely produced in industry. However, PZT piezoelectric ceramics pollute the environment and damage the body in the production process，and its piezoelectric performance is limited in high temperature fields [6,7]. Therefore, lead-free piezoelectric ceramics have become a hot spot in current research. The Curie temperature of K_0.5Na_0.5NbO₃ and Bi_0.5Na_0.5TiO₃ based ceramics are far from satisfying the application of high temperature fields [8-10]. Lead-free piezoelectric ceramics with bismuth layered are usually utilized in higher temperature fields, but the piezoelectric properties are lower [11,12].

BiFeO₃ is a twisted trigonal perovskite structure with high Curie temperature. The BiFeO₃-BaTiO₃ (BFBT) binary system shows high T_C in the components of the rhombohedral and pseudocubic phase boundaries [13]. Related studies have reported the influence of Mn doped on BFBT ceramics, and obtained the piezoelectric ceramics with d₃₃= 169 pC/N, T_C = 506℃, T_d = 500℃, tanδ ≈ 4.4% [14]. Bi(Zn_0.5Ti_0.5)O₃ (BZT) is a Bi-based perovskite compound, the large residual polarization and high tetragonality are P_r > 150 μC/cm² , c/a = 1.21, respectively [15]. BFBT-BZT+MnO₂ ternary solid solution reduces the dielectric loss and improves the temperature stability of ceramics [16-18]. Li₂CO₃ is a conventional sintering aid, when Li₂CO₃ was added into ceramics, which promotes ceramic sintering and makes BFBT-BZT+MnO₂ ceramics dense [19-22].

However, in the sintering process, Bi₂O₃ is volatile and the change of Fe³⁺ into Fe²⁺ in BiFeO₃ caused a number of oxygen vacancies in ceramics [23]. This phenomenon makes less compact sintering of ceramics. Therefore, the stoichiometric ratio of BF/BT in ceramics became the focus of the experiment. So, the experiment made the ceramics dense by changing the contents of BF and BT, and it was believed that the piezoelectric properties can still be improved, and the low dielectric loss can be obtained of the ceramics. In this paper, (1-x)BiFeO₃-xBaTiO₃-0.025Bi(Zn_0.5Ti_0.5)O₃+0.0035MnO₂+0.003Li₂CO₃ (where x = 0.24, 0.26, 0.28, 0.30, 0.32, 0.34 mol%, abbreviated as (1-x)BF-xBT-BZT) lead-free piezoelectric ceramics were prepared by solid phase sintering. The phase transition, microstructure, electrical properties, Curie temperature and depolarization temperature of the ceramics were investigated experimentally. After a series of studies, the ceramics obtained with high piezoelectric properties and high Curie temperature in morphotropic phase boundary (MPB). Related studies are listed in Table 1 and Table 2.

The (1-x)BF-xBT-BZT ceramics were made by solid-state reaction method using Bi₂O₃, Fe₂O₃, BaCO₃, TiO₂, ZnO, MnO₂, and Li₂CO₃ as raw materials, the purity of all raw materials is more than 99%. The dried raw material powders were prepared in proportion and then ball milled for 24 h by alcohol. After that, the raw materials were dried, sieved and then calcined at 780 ℃ for 4 h. The powders synthesized after sintering was ball milled again then dried. The powders were mixed with 8 wt% PVA and dried, raw plain disks with a diameter of 12 mm were made under 10 MPa. Finally, all samples were sintered at 960-1000℃ for 2-8 h. After the above steps, the crystal structure and phase transformation of the ceramics were analyzed by X-ray diffraction analysis, referred to as XRD (D8-2-Advanced, Bruker AXS, Germany). This experiment used scanning electron microscopy (SEM, JSM-5610LV, JEOL, Japan) to observe the microstructure of ceramic samples. And the experiment measured the piezoelectric constant by d₃₃ quasi-static instrument (ZJ-3A, CAS, Shanghai, China). For the planar electromechanical coupling factor k_p and mechanical quality factors Q_m were determined through precision impedance analyzer (4294A, Agilent Company). The polarization hysteresis loop was tested by a ferroelectric tester (Premier II, Radiation Technology Corporation, Albuquerque, NM, USA). Dielectric temperature spectrum of samples at room temperature to 700℃ was measured by dynamic impedance analyzer (Agilent 4294A). The non - in - situ method measured the depolarization temperature of samples in this experiment.

Fig. 1 shows the XRD patterns of (1-x)BF-xBT-BZT ceramics samples. The main structure of all samples is ABO₃-type perovskite structure. This phenomenon shows that the ceramics have formed a homogeneous ternary solid solution [35,36]. In order to descript the phase structure transition of the ceramics more carefully, the characteristic peak near 39˚ are enlarged as displayed in Fig. 1(b). When the content of BaTiO₃ increases from 0.24 to 0.34, the characteristic peak evolved from the double peak (003 and 021) to a single peak (111). The shift is mainly near x = 0.3. When the range of x is 0.24-0.28, the phase structure of ceramics is rhombohedral. When x ≥ 0.32, the phase structure converted to pseudocubic phase. The rhombohedral and the pseudocube phase coexist when x is around 0.3, the existence of MPB in 0.7BF-0.3BT-BZT sample [25,27,37].

Fig. 2-1 is the surface microstructures of (1-x)BF-xBT-BZT ceramics sintered at 980℃. Fig. 2-2 is the average grain size distributions of the ceramics. All samples have no obvious holes, which could be reflected in the SEM micrographs of different BT contents. When x = 0.24, the average grain size of ceramics is relatively larger. With the content of BT increases, the grain size of the ceramics decreases significantly. When x ≥ 0.28, the grain sizes don’t become smaller anymore and tend to be stable. The reason for this phenomenon is that BF is a low-melting material [38]. At the same sintering temperature, more BF promotes grain growth and reduces sintering temperature. Furthermore, with the increase of BT, the oxygen vacancies decrease during BF sintering process (the change of Fe³⁺ to Fe²⁺ and the volatility of Bi₂O₃) [23,32,39], which is not conducive to grain transfer, and ultimately inhibits grain growth [40]. It is worth noted that the liquid phase appears clearly at x = 0.3, which indicates that the BF and BT content reaches the optimal ratio and promoted sintering.

Fig. 3 presents the variation trend of piezoelectric constant d₃₃, electromechanical coupling coefficient k_p, mechanical mass factor Q_m and dielectric loss tanδ with BT content. The d₃₃ and k_p increase first and reach the maximum d₃₃ = 184 pC/N, k_p = 0.335 at x = 0.3, then decrease with the change of BT. The tanδ increases and the Q_m shows a downward trend with the rise of x, tanδ = 1.9 % and Q_m = 72.71 respectively at x = 0.24. According to the XRD results, the phase structure in the MPB range is formed near x = 0.3 of the sample. For the ceramic with the MPB structure, the drive energy required for the domain wall movement of the ceramics is lowered, and the domain activity is increased so the piezoelectric property can be improved remarkably [25,41,42]. The main reason for the decrease of Q_m and the increase of tanδ is that with the BT content increases, the oxygen vacancies decrease due to the change of Fe³⁺ to Fe²⁺. Furthermore, the reduction of oxygen vacancies makes it easier to turn the domain, which makes tanδ increase, Q_m decrease and increases the aging rate of ceramics.

At room temperature, the P-E hysteresis loop are depicted as Fig. 4, and P, E, P_r, E_c represent polarization intensity, applied electric field, residual polarization intensity and coercive field, respectively. The used electric field in ferroelectric behavior test is from 30 kV/cm to 60 kV/cm. From the Fig. 4, typical ferroelectric polarization hysteresis loops were shown. Except for x = 0.24, the remaining ceramics samples are in a relatively saturated state when E is 60 kV/cm. As we can see from Fig. 4(g) when x rises from 0.24 to 0.26, P_r and E_c increase significantly. P_r slowly increases to a maximum 20.13 μC/cm² at x = 0.34, the E_creaches 33.77 kV/cm which is the maximum value at x = 0.26 and then it shows a decreasing trend. The reason why P_r increases is that favorable uniformity of grain size and the improving densification of structure with the increase of BT content, which means the more completed polarization and stronger ferroelectric properties. The sudden increase for E_c is caused by the decrease in grain size when x = 0.24 to 0.26. The increase of grain boundaries makes it difficult to flip the domain [16,17,18], the P_r becomes larger slightly, but E_c becomes smaller as the grain continues to decrease. It is noted in Fig. 4(e-f) that the hysteresis loop is not smooth under the E of 60 kV/cm, this is because the high electric field caused the ceramic sample to leak current [14,16].

Fig. 5(a-f) shows the e_r and tanδ of all samples, e_r represents dielectric constant and tanδ represents loss tangent. The frequencies are 1 kHz, 10 kHz and 100 kHz, respectively. All ceramic samples have good temperature dependence from room temperature to 700℃. The e_r varies little when the temperature increase at the beginning, it rapidly increases to the peak at a certain temperature (T_c), and finally decreases. As shown in Fig. 5(g), T_c reaches the maximum of 580℃ when x = 0.24, and Curie temperature reduces with the increase of BT. The tanδ increases before reaching the T_c when the rang of x is 0.24 to 0.28. And the tanδ decreases at the Curie point, increases again with the temperature increases. When x ≥ 0.30, the tanδ increases rapidly after Curie point decreases.

According to the modified Curie-Weiss law:

where the curve of ln(1/e_r − 1/e_m) as a function of ln(T − T_m) for the ceramics, which are presented in Fig. 5(h). In the formula, e_m is the maximum value of e_r, T_m denotes phase transition temperature, C is Curie-like constant and γ is degree of diffuseness. Furthermore, the range of γ is from 1 to 2, where 1 represents a normal ferroelectric, 2 represents ideal relaxor ferroelectric [29]. It can be seen from Fig. 5(a-f), all (1-x)BF-xBT-BZT ceramics are relaxor ferroelectrics. Under the T_c, with the increase of frequency (1 kHz to 100 kHz), the e_r decreases, the tanδ generates (x < 0.30), the dielectric peak and the loss peak move toward the high temperature, all of which are caused by the frequency dispersion characteristics of relaxation ferroelectrics [16]. Above the T_c, the tanδ of the samples increase again because the ceramics have a slight leakage current at high temperature. With the increase of x, the Curie temperature reduces, which is due to the increase of dielectric loss at room temperature which caused by oxygen vacancy in the sintering process. It is worth noting that when x < 0.3, with the frequency increases, the e_r decreases before the Curie point. And when x ≥ 0.3, the loss peak disappears, which is due to the reason that the frequency dispersion of the relaxed ferroelectric weakened. The trend of e_r and tanδ for all (1-x)BF-xBT-BZT samples is consistent with γ of relaxation ferroelectrics.

The depolarization curve of the (1-x)BF-xBT-BZT ceramics is depicted in the Fig. 6. The d₃₃ of the samples as a function of temperature was measured by ex - situ d₃₃ method. With the increase of temperature, there is no obvious change for d₃₃. When a certain temperature (T_d) arrives, the d₃₃ drops suddenly [26,43]. For ceramic samples with x = 0.24, when the depolarization temperature is 550℃, d₃₃ = 85 pC/N. When x = 0.3 and T_d = 530℃, the d₃₃ is still as high as 150 pC/N. The figure shows that depolarization law of all ceramic samples is consistent with the variation of the Curie temperature as Fig. 5(g). When the BT content ranges from 0.24 to 0.34, the decrease of depolarization temperature is due to the increasing loss for the ceramics, as described in Fig. 3(b). When x = 0.3, the high d₃₃ is caused by the ceramic at MPB.

The (1-x)BF-xBT-BZT ceramics were synthesized by solid-state sintering method. The effect of BT as a variable on the structure, micromorphology, piezoelectric, ferroelectric properties and Curie temperature of ceramics was investigated. The XRD analysis results indicate that the rise of BT can cause a phase transformation from rhombohedral to pseudocubic phase. The (1-x)BF-xBT-BZT system has a MPB at x = 0.3. And the 0.7BF-0.3BT-BZT ceramics exhibit the best d₃₃= 184 pC/N, and high T_c = 550℃, particularly when T_d = 530℃, d₃₃ = 150 pC/N. It is worth pointing out that the 0.76BF-0.24BT-BZT ceramic has excellent Curie temperature T_c= 580℃, and low dielectric loss tanδ = 1.9 %. The high electrical properties and improved temperature stability demonstrates that the ceramics we prepared can be used effectively in high temperature field.

Acknowledgements

This work was supported by the National Nature Science Foundation of China (11664006 and 11364008), Natural Science Foundation of Guangxi (2014GXNSFAA118311), and Guangxi Key Laboratory of Information Materials.

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Table 1. d₃₃, T_C, and T_d of the reported piezoelectric ceramics.

Systems	d₃₃(pC/N)	T_c (℃)	T_d (℃)
0.35BiScO₃-0.6PbTiO₃-0.05(Zn_1/3Nb_2/3)O₃[24]	470	420	260
0.725BiFeO₃-0.275BaTiO₃ [25]	136	485	420
0.71BiFeO₃-0.29BaTiO₃+1.0 mol%MnO₂[14]	140	512	500
(1−x)BiFeO₃-xBaTiO₃+0.4wt%CuO+0.6wt%MnO₂[26]	170	485	480
0.725BiFeO₃-0.275BaTiO₃+0.35mol%MnO₂+0.3mol%Li₂CO₃[21]	163	508	480
0.72BiFe_0.99Al_0.01O₃-0.28BaTi_0.97Zr_0.03O₃ [27]	157	435	425
0.71BiFeO₃-0.29BaTi(Mg_1/3Nb_2/3)O₃ [28]	158	453	400
0.71BiFe_0.9(Zn_1/2Ti_1/2)_0.1O₃-0.29BaTiO₃ [16]	163	428	380
0.75BiFeO₃-0.25BaTiO₃-0.01NdCoO₃+1mol%MnO₂[29]	110	605	525
0.7BiFeO₃-0.3BaTiO₃-0.025Bi(Zn_0.5Ti_0.5)+0.003MnO₂+0.003Li₂CO₃ [22]^{Our work}	184	554	530
0.76BiFeO₃-0.24BaTiO₃-0.025Bi(Zn_0.5Ti_0.5)O₃+0.0035MnO₂+0.003Li₂CO₃^{This work}	102	580	550

Table 2. d₃₃, T_C, and T_d of the reported BF-BT-BZT piezoelectric ceramics.

BF-BT-BZT System	d₃₃(pC/N)	T_c (℃)	T_d (℃)
0.71BiFe_0.9(Zn_1/2Ti_1/2)_0.1O₃-0.29BaTiO₃+0.6wt%MnO₂ [17]	163	428	380
0.65BiFeO₃-0.30BaTiO₃-0.05Bi(Zn_0.5Ti_0.5)O₃+1mol%MnO₂ [30]	139	565	-
0.97[0.67Bi_1.05FeO₃-0.33BaTiO₃]-0.03Bi_1.05(Zn_0.5Ti_0.5)O₃ [31]	324	466	-
0.696BiFeO₃-0.014Bi(Zn_0.5Ti_0.5)O₃-0.28BaTiO₃+0.26wt%MnO₂ [32]	147	514	-
0.99[0.715BiFeO₃-0.285BaTiO₃]-0.01Bi(Zn_0.5Ti_0.5)O₃ [33]	195	505	400
0.67BiFeO₃-0.33BaTiO₃-0.03Bi(Zn_0.5Ti_0.5)O₃+0.0035MnO₂+0.004CuO [18]	188	420	426
0.7BiFe_0.95-0.05(Zn_0.5Ti_0.5)_0.03O₃-0.3BaTiO₃ [34]	135	482	-
0.98[0.60BiFeO₃-0.40BaTiO₃]-0.02Bi_1.05(Zn_0.5Ti_0.5)O₃[16]	50	350	-
0.7BiFeO₃-0.3BaTiO₃-0.025Bi(Zn_0.5Ti_0.5)+0.0035MnO₂+0.003Li₂CO₃[22]^{Our work}	184	554	530
0.76BiFeO₃-0.24BaTiO₃-0.025Bi(Zn_0.5Ti_0.5)O₃+0.0035MnO₂+0.003Li₂CO₃^{This work}	102	580	550

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published 11 Jul, 2021

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The (1-x)BiFeO3-xBaTiO3-Bi(Zn0.5Ti0.5)O3 high temperature lead-free piezoelectric ceramics with strong piezoelectric properties

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1. Introduction

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3. Results And Discussion

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