Research Article pubs.acs.org/journal/ascecg
Cite This: ACS Sustainable Chem. Eng. 2017, 5, 10215-10222
Novel Strontium Titanate-Based Lead-Free Ceramics for High-Energy Storage Applications Haibo Yang,* Fei Yan, Ying Lin, and Tong Wang School of Materials Science and Engineering, Shaanxi University of Science and Technology, 710021, Weiyang District, Xi’an, China ABSTRACT: To achieve the miniaturization and integration of advanced pulsed power capacitors, it is highly desirable to develop lead-free ceramic materials with high recoverable energy density (Wrec) and high energy storage efficiency (η). Whereas, Wrec (2 J/cm3) and high η (>80%), simultaneously, because of large Pr and low BDS.19,20 For instance, Shen et al. reported that a Wrec of 0.71 J/cm3 and a η of 71.5% could be obtained at 93 kV/cm in 0.91BaTiO30.09BiYbO 3 ceramic. 21 Xu et al. obtained the 0.90(0.92Bi0.5Na0.5TiO3-0.08BaTiO3)-0.10NaTaO3 ceramic with a Wrec of 1.2 J/cm3 and a η of 74.8% at 100 kV/cm.22 Recently, Wang et al. reported that the [(Bi 0.5 Na 0.5 ) 0.94 Ba 0.06 ]La(1−x)ZrxTiO3 ceramics have double P−E hysteresis loops, small Pr, and large Pmax (37.5 μC/cm2), but the BDS is too low to obtain high energy storage properties (the maximum value of Wrec is only 1.58 J/cm3).23 KNN-based ceramics are more beneficial to be used for advanced pulsed power capacitors due to high Wrec (∼4 J/cm3), but their value of η are lower than 65% because of larger Pr. A Wrec of 4.03 J/cm3 and a η of 52% were achieved for 0.85(K0.5Na0.5)NbO3-0.15SrTiO3 ceramic.24 Dielectric materials with lower η lose a higher amount of their stored energy to heat, and the generated heat would degrade the properties of dielectric materials.25 Meanwhile, the cost of raw materials for KNN-based ceramics is too expensive to be commercialized, and it is difficult to obtain KNN-based ceramics because the sintering temperature range of KNN ceramics is extremely narrow.26−28 Therefore, for lead-free energy storage ceramic materials not only the excellent properties but also the cost and feasible mass-production
fabrication process should also been considered. SrTiO3 (ST) needs relatively inexpensive raw materials, has a broad sintering temperature range, and can be used for mass-production for high-voltage capacitors.29 In addition, ST-based ceramics are also expected to be used for high energy storage capacitors. Because ST possesses unique physical properties, for instance, low dielectric loss ( 80%. Therefore, the (1−x)ST-x(BNTBLZT) (x = 0−0.5) ceramics can be used for high energy storage applications.
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EXPERIMENTAL SECTION
Materials Preparation. The (1−x)ST-x(BNT-BLZT) (x = 0.0− 0.5) lead-free ceramics were fabricated using the tape-casting process and sintered by solid-state sintering method. First, ST and BNT-BLZT powders were synthesized, respectively. SrCO3 (>99.0%) and TiO2 10216
DOI: 10.1021/acssuschemeng.7b02203 ACS Sustainable Chem. Eng. 2017, 5, 10215−10222
Research Article
ACS Sustainable Chemistry & Engineering (>99.8%) were weighed by the nominal composition of ST and ball milled in alcohol for 12 h. The obtained powders were dried and calcined at 1150 °C for 4 h in air, and then milled again in alcohol for 12 h. Bi2O3 (>99%), Na2CO3 (>99.8%), TiO2 (>99.8%), BaCO3 (>99.0%), La2O3 (>99.9%), and ZrO2 (>99%) were the raw materials of BNT-BLZT powders. The preparation process was as same as that of ST powders, except that BNT-BLZT powders were calcined at 800 °C for 4 h. BNT-BLZT and ST powders were mixed according to the composition of (1−x)ST-x(BNT-BLZT) and ball-milled in alcohol for 12 h. After drying, the (1−x)ST-x(BNT-BLZT) mixture powders can be obtained. To get the slurries, dispersant (glycerol trioleate) and solvent (alcohol and butanone) were milled for 4 h. Then some plasticizer (dibutyl phthalate), binder (polyvinyl butyral and polyethylene glycol), and (1−x)ST-x(BNT-BLZT) powders were added and milled for 4 h again. Finally, the obtained slurries were casted on Mylar substrates. The schematic drawing of the fabrication process are shown in Figure 2. The ceramic membrane was laminated first and uniaxially pressed under 120 MPa at room temperature. And then, heating at 80 °C and pressing under 200 MPa again. Finally, binders were removed at 550 °C for 24 h, and all the samples were sintered at 1300−1350 °C for 2 h. To prevent the loss of volatile Bi3+ and Na+, the samples were embedded in the corresponding powders during sintering. Characterization. The X-ray diffractometer (XRD, D-MAX 2200pc, Rigaku Co., Tokyo, Japan) was used to detect phase structure of (1−x)ST-x(BNT-BLZT) ceramics. The microstructure of (1− x)ST-x(BNT-BLZT) ceramics was observed by a scanning electron microscopy (SEM, S4800, Rigaku Co., Japan). The frequency dependent dielectric properties were measured by an impedance analyzer (E4990A, Agilent, Palo Alto, CA). The temperaturedependent dielectric properties were measured using an LCR meter (3532-50, Hioki, Ueda, Japan) at a frequency of 1 kHz. The P−E loops were measured by a ferroelectric test system (Premier II, Radiant, USA) and the samples with a thickness of 0.20 mm.
Figure 4. SEM of (1−x)ST-x(BNT-BLZT) ceramics: (a) x = 0; (b) x = 0.1; (c) x = 0.2; (d) x = 0.3; (e) x = 0.4; and (f) x = 0.5.
Measurer), as shown in Figure 5a−f. It can be found that the average grain size increases from 1.09 to 4.86 μm with increasing BNT-BLZT content. The increase of grain size might be the result of the A-site elements (Bi3+ and Na+) volatilizing inevitably because of their low melting points,22,38 leading to the presence of oxygen vacancies and promoting mass transportation during sintering.39 Figure 6 shows the frequency dependent dielectric constant (ε′) and dielectric loss (tan δ) for (1−x)ST-x(BNT-BLZT) ceramics. It can be found that the ε′ almost remains a constant with measurement frequency when x ≤ 0.4, and then an excellent frequency stability of ε′ can be observed. In addition, the ε′ of (1−x)ST-x(BNT-BLZT) ceramics increases with increasing BNT-BLZT content gradually. It is because, compared with ST, BNT-BLZT has larger ε′ and higher Curie temperature (TC).23,40 Meanwhile, all the samples keep a low value of tan δ ( 80%.
Figure 12. (a) Unipolar P−E loops of 0.8ST-0.2(BNT-BLZT) ceramics with different electric fields at room temperature. (b) Calculated W and Wrec from panel a. (c) Calculated Wloss and η from panel a.
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CONCLUSIONS In this study, novel ST-BNT-BLZT lead-free ceramics were successfully fabricated by the tape-casting process and sintered via solid-state sintering method for achieving large Pmax, high BDS, high Wrec, and high η. All the samples have slim P−E loops. The Pmax gradually increases and reaches the maximum value of 28.44 μC/cm2 for the sample with x = 0.5 at 160 kV/ cm, which is 4.44 times as large as that of pure ST (6.40 μC/ cm2). A high Wrec (2.83 J/cm3) and high η (85%) can be
Figure 13. A comparison of η and Wrec between (1−x)ST-x(BNTBLZT) ceramics and other lead-free ceramics.
simultaneously achieved for 0.8ST-0.2(BNT-BLZT) ceramic at 320 kV/cm. The significantly enhanced Wrec (2.83 J/cm3) is almost 2 times higher than previous reported results of lead-free ceramics with η > 80%, which indicates that the (1−x)ST10220
DOI: 10.1021/acssuschemeng.7b02203 ACS Sustainable Chem. Eng. 2017, 5, 10215−10222
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x(BNT-BLZT) ceramics can be considered as potential candidate ceramic capacitors for high energy storage applications. In addition, the finding in this study could push the development of ST-based ceramics with enhanced Pmax, high Wrec, and high η in the future.
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AUTHOR INFORMATION
Corresponding Author
*E-mail:
[email protected]. ORCID
Haibo Yang: 0000-0003-1828-3750 Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS This work is supported by the National Natural Science Foundation of China (Grant No. 51572159, 51702196), the Chinese Postdoctoral Science Foundation (Grant No. 2016M590916), the Science and Technology Foundation of Weiyang District of Xi’an City (Grant No. 201605), the Industrialization Foundation of Education Department of Shaanxi Provincial Government (Grant No. 16JF002).
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DOI: 10.1021/acssuschemeng.7b02203 ACS Sustainable Chem. Eng. 2017, 5, 10215−10222
