Startseite Fabrication and performance of PNN-PZT piezoelectric ceramics obtained by low-temperature sintering
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Fabrication and performance of PNN-PZT piezoelectric ceramics obtained by low-temperature sintering

  • Jing Zhang , Yuansong Zhang EMAIL logo , Zhoumin Yan , Anjiu Wang , Ping Jiang und Min Zhong
Veröffentlicht/Copyright: 7. November 2020
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Science and Engineering of Composite Materials
Aus der Zeitschrift Science and Engineering of Composite Materials Band 27 Heft 1

Abstract

The Pb(Ni1/3Nb2/3)O3-Pb(ZrxTi1−x)O3 (PNN-PZT) piezoelectric ceramics with CuO and LiBiO2 doping were successfully fabricated by the low-temperature solid-state reaction to effectively restrain the PbO volatilization. The microstructure and electrical properties of the PNN-PZT ceramics were characterized. The experimental results reveal that the PNN-PZT ceramics are composed of a pure perovskite structure in which the rhombohedral and tetragonal phases coexist. Meanwhile, the good electric properties, including low dielectric loss, outstanding diffusion phase transition and palpable dielectric relaxation, are exhibited in PNN-PZT ceramics with 0.2 wt.% CuO and 1 wt.% LiBiO2 addition. This piezoceramic composition possibly provides a reference for the application of multi-layer piezoelectric actuators.

Keywords: piezoelectric ceramics; low-temperature sintering; electric properties; dielectric relaxation

1 Introduction

With the rapid development of the electronic information technology, the electronic components widely applied in various devices, such as transformers, reproducers and filters, trend to be smaller, lighter and cheaper [1, 2, 3]. As the most popular lead-based piezoelectric ceramic, The PNN-PZT system with excellent piezoelectric constant, high electromechanical coupling factor and eminent permittivity are widely used both in military and civilian applications [4, 5]. As is known, the sintering temperature of PNN-PZT ceramic is about 1200 ~ 1300∘C [6]. The strong volatilization of lead oxide beyond 960∘C in the conventional solid-state reaction can deteriorate the electrical properties of samples [7]. Moreover, the lead is one of heavy metals which are extremely harmful for human health [8]. Additionally, the PbO volatilization in the co-fire of PNN-PZT ceramic and Ag-Pd electrode can substantially improve the crack formation in the multi-layer piezoelectric actuators. Currently, the most common approach to slow the volatilization of PbO is sintering in a hermetic atmosphere and adding an excessive amount of PbO, however this problem is not solved efficiently. Thereby, the adjustable sintering temperature (below 960∘C), which can postpone availably the volatilization of PbO and promote the energy saving, has aroused the extensive concerns [9, 10, 11].

The research on the low-temperature sintering of piezoelectric ceramics has been developed for decades [12]. Generally, there are two methods to reduce the sintering temperature. One is refining effectively the particle size of powders. The ceramic powders prepared by sol-gel methods or hydrothermal process possess superfine particle sizes and high surface energy, which can indeed reduce the sintering temperature [13]. Besides, the another one is adding tiny amounts of efficacious sintering aids, such as V2O5, SiO2, etc, which is an economic and efficient approach to reducing the sintering temperature. The sintering aids are conducive to forming low-melting-point glass phases during the solid reaction. The glass phase formed in the grain boundary accelerates the rate of atomic migration, which is contribute to fast growth of grains. The studies showed that moderate B2O3 and CuO doped (Ba, Ca)(Ti, Sn)O3 can reduce the sintering temperature from1250∘C to 1200∘C. Furthermore, the introduction of a tiny amount of low-melting frit (B2O3-Bi2O3-CdO) can reduce the sintering temperature even to 960∘C.

Commonly, the electrical properties of piezoelectric ceramics could be deteriorated when the sintering temperature reduced improperly [14, 15]. Therefore, on the basis of ensuring that Ag layer is not melted (~960∘C), obtaining high-performance piezoelectric ceramic materials is a key scientific problem to be solved urgently in the development of piezoelectric actuators. As is known, the PNN-PZT ceramic is a typical "soft material", which exhibits a relatively low sintering-temperature and excellent electrical properties. Introduction of CuO and Bi2O3 into the PNN-PZT ceramics as the sintering aids can reduce effectively the sintering temperature [16, 17, 18]. Therefore in this notion, a series of PNN-PZT ceramics doped by various amounts of CuO and LiBiO2 as sintering aids to achieve a novel electric properties via low-temperature sintering. Thereinto, the LiBiO2 can be synthesized by Li2CO3 + Bi2O3 = 2LiBiO2 + CO2. The effect of varying contents of sintering aids on the microstructure and electrical performances were carefully investigated. The related research results will provide a potential candidate for the multi-layer piezoelectric actuators.

2 Material and experimental procedures

2.1 Piezoceramic preparation

The 0.3 Pb(Ni1/3Nb2/3)O3-0.7 Pb(Zr0.41Ti0.59)O3+x wt.% CuO+y wt.% LiBiO2+1 wt.% Pb3O4 (x = 0.1, 0.2, 0.3, y = 1, 2) piezoelectric ceramics were fabricated by traditional solid-state reaction technique. The Pb3O4, ZrO2, TiO2, Nb2O5, NiO, CuO, Bi2O3 and Li2CO3 powders with a purity of more than 99.9% were used as the raw materials. The powders were weighed by an electronic balance of 0.1mg (AL204), and then blended with alcohol by ball-milling in a nylon jar for 12 h at 300 rpm. Subsequently, the mixed powders were dried and calcined at 900∘C for 2h. After addition of CuO, Li2CO3 and Bi2O3, the pre-sintered powders were ball-milled again with alcohol and dried. Hereafter, these powders mixed with 5 wt.% PVA as binder were pressed under 12 MPa into a planchette whose size is Ф10 mm×1 mm. Besides, the ceramics were sintered at 960∘C in air for 2 h. And then the sintered samples were printed on both sides with sliver electrodes at 850∘C. Finally, the samples for piezoelectric measurements were poled at 70∘C in silicone oil by applying a DC electric field of 3 kV·mm−1 for 20 min.

2.2 Piezoceramic characterization

The phase composition of samples was measured by a X’pert-PRO X-ray diffractometer (XRD). The microstructure was observed by a Supra-40 scanning electron microscopy (SEM, Germany). The piezoelectric constant (d33) was tested at room temperature using a quasi-static piezo-d33 meter (ZJ-3A, China), in which at least 10 times were conducted to obtain the average value. The dielectric properties were characterized using an LCR meter (Agilent, E4980A), connected to a computer-controlled temperature chamber, by measuring at 10 kHz.

3 Results

3.1 Phase identification of PNN-PZT ceramics

Figure 1 shows the XRD patterns of PNN-PZT+ x CuO+ y LiBiO2 ceramics with various amounts of CuO, Li2CO3 and Bi2O3 addition. Clearly, all the specimens exhibit a single perovskite structure (ABO3).No intermediate phases, such as pyrochlore or Zr and Ti-rich phases, was found, indicating that CuO and LiBiO2 could have solved completely into the perovskite solid solution, rather than concentrated in the grain boundaries.Meanwhile, the peak around 45o has been split into two ones: the right one (R) is (002) and the left (T) is (200) preferred orientation, indicating the coexistence of the rhombohedral (R) and the tetragonal phase (T) inPNN-PZT piezoelectric ceramics. It has been reported that the interface between R and T phases is perfectly located in morphotropic phase boundary (MPB), possessing the excellent piezoelectric properties [19, 20].

Figure 1 X-ray diffraction patterns of PNN-PZT + xwt.% CuO + ywt.% LiBiO2 + 1wt.% Pb3O4 ceramics with different amounts of CuO, Li2CO3 and Bi2O3.
Figure 1

X-ray diffraction patterns of PNN-PZT + xwt.% CuO + ywt.% LiBiO2 + 1wt.% Pb3O4 ceramics with different amounts of CuO, Li2CO3 and Bi2O3.

3.2 Microstructure of PNN-PZT ceramics

Figure 2(a) ~ (d) shows the microstructure of PNN-PZT-xCuO-yLiBiO2 piezoelectric ceramics. It is suggested that the grains are relatively small and many pores exist while the sintering aids short supplied. However, with the increase of sintering aids, the grains grow gradually and the density and homogeneity of ceramics get better, particularly in the PNN-PZT- 0.1% CuO- 2% LiBiO2 ceramic. It demonstrates that moderate CuO and LiBiO2 additions could enhance the grain growth and increase the densification. Nevertheless, as the dopant successively increases, the CuO and LiBiO2 will aggregate at the grain boundary and cannot dissolve completely into crystal lattices as shown in Figure 2 (c), causing that the overall electric performance gets worse.

Figure 2 Microstructures of PNN-PZT-xCuO-yLiBiO2 ceramics. (a) x = 0.1, y = 1; (b) x = 0.1, y = 2; (c) x = 0.2, y = 1; (d) x = 0.2, y = 2.
Figure 2

Microstructures of PNN-PZT-xCuO-yLiBiO2 ceramics. (a) x = 0.1, y = 1; (b) x = 0.1, y = 2; (c) x = 0.2, y = 1; (d) x = 0.2, y = 2.

3.3 Electric properties of PNN-PZT ceramics

Table 1 shows the electrical properties of PNN-PZT+xCuO +yLiBiO2 ceramics. As is seen from Table 1, the changes of kp and d33 possess the same tendency and reach the maximum values when x = 0.2, y = 1. They are 608 pC·N−1 and 0.65 respectively. Meanwhile, the relative permittivity (єr) reaches 3843 and the loss (tan δ) is approximately equal to 2.19%. That means, the upper density, good homogeneity and few second phases (in the sample 3#) are significantly helpful for improving the electric properties of ceramics.

Table 1

Electric properties of PNN-PZT ceramics.

Compositionkpd33 (pC·N−1)tan δ (%)єr
x = 0.1, y = 10.514902.343228
x = 0.1, y = 20.545512.623789
x = 0.2, y = 10.656082.193843
x = 0.2, y = 20.484702.513277
x = 0.3, y = 10.434402.743412
x = 0.3, y = 20.414102.713220

3.4 Dielectric properties at various temperatures of PNN-PZT ceramics

Figure 3 shows the temperature dependence of dielectric constant and loss of PNN-PZT ceramics with different contents of CuO and LiBiO2 measured at 100 kHz. As can be seen from Figure 3 (a), the phase-transition peaks of ferroelectric and paraelectric are observed in all ceramics, which corresponds to the Curie temperature (Tc). Obviously, the Tc reduced with the increasing of LiBiO2 contents. However, the content of CuO is helpful for the increasing of Tc and the reduction of tan δ. The ceramic with 0.2 wt.% CuO and 1wt.% LiBiO2 possesses the highest Tc of 191.6∘C, and the lowest loss of 2.19%, respectively.

Figure 3 Temperature dependence of (a) єr and (b) tan δ of PNN-PZT ceramics with different contents of CuO and LiBiO2 measured at 100 kHz.
Figure 3

Temperature dependence of (a) єr and (b) tan δ of PNN-PZT ceramics with different contents of CuO and LiBiO2 measured at 100 kHz.

3.5 Relaxation behavior of PNN-PZT ceramics

Figure 4 shows the relationship between inverse dielectric constant and temperature of PNN-PZT+x CuO+y LiBiO2 ceramics at 10 kHz. The permittivity of the ferroelectric materials calculated according to the Curie-Weiss law when the temperature is beyond Tc, as shown in Eq. (1) [12]:

Figure 4 Inverse permittivity as a function of temperature for ceramics at 100 kHz (a) x = 0.1, y = 1; (b) x = 0.1, y = 2; (c) x = 0.2, y = 1; (d) x = 0.2, y = 2.
Figure 4

Inverse permittivity as a function of temperature for ceramics at 100 kHz (a) x = 0.1, y = 1; (b) x = 0.1, y = 2; (c) x = 0.2, y = 1; (d) x = 0.2, y = 2.

(1)ϵ=CT−Tcw

where Tcw represents the Curie-Weiss temperature and C is the Curie-Weiss constant. The deviation degree of Curie transition can be described in Eq. (2) [12]:

(2)ΔTm=TB−Tm

where ΔTm is the deviation, TB is the initial temperature that the dielectric materials obey the Curie-Weiss law, and Tm refers to the temperature corresponding to the maximum of permittivity. It can be seen from Figure 4 that PNN-PZT ceramic belongs to a typical relaxor ferroelectric. The ceramics with fewer LiBiO2 contents exhibits a higher ΔTm than that of ceramic with 2 wt.% LiBiO2 additions. Hence, the appropriate addition of LiBiO2 can lower the sintering temperature, thus enhancing the relaxation behavior of piezoelectric ceramics.

The plots of ln(1/єr −1/єm)/ ln(T −Tm) for PNN-PZT+x CuO+y LiBiO2 ceramics measured at 100 kHz are shown in Figure 5. The dispersion coefficient γ can be obtained by linear fitting of Eq. 2. The ceramic will be a normal ferroelectric when γ is equal to 1, but will transform into imperfect relaxor ferroelectric when γ is ranged from 1 to 2.

Figure 5 Plot of ln(1/єr − 1/єm)/ ln(T − Tm) for ceramics at 100 kHz (a) x = 0.1, y = 1; (b) x = 0.1, y = 2; (c) x = 0.2, y = 1; (d) x = 0.2, y = 2.
Figure 5

Plot of ln(1/єr − 1/єm)/ ln(T − Tm) for ceramics at 100 kHz (a) x = 0.1, y = 1; (b) x = 0.1, y = 2; (c) x = 0.2, y = 1; (d) x = 0.2, y = 2.

When γ = 2, the ceramic will become a relaxor ferroelectric with diffuse phase transition. It is observed from Figure 5 that the γ increases firstly with the increase of LiBiO2 concentration, especially for the PNN-PZT ceramic modified with 1wt.%CuO and 2wt.%LiBiO2, the γ is approach to 2.036 at 100 Hz, which means that the PNN-PZT ceramic modified with 1wt.%CuO and 2wt.%LiBiO2 is an excellent relaxor ferroelectric.

4 Discussion

Universally, the improvement of dielectric constant (d33) is closely related to the formation of Pb-ion vacancies to effectively promote the domain rotation. The extensive additions of Bi3+ introduced into the ceramics substitute for the Pb-sites, also result in many Pb2+ vacancies to keep the electrical neutrality. In this study, the adjustable amounts of sintering aids were dissolved into the perovskite solid solution, further leading to the increase of d33. However, the excessive additions of sintering aids could segregate in the grain boundaries to pin the domain rotation, further decreasing the value of d33. Besides, the LiBiO2 and CuO added to the PNN-PZT ceramics are much beneficialfor achieving a dense and uniform microstructure, which was also helpful to obtain a prominent d33 improvement.

To comprehensively evaluate the piezoelectric properties of the PNN-PZT ceramics with CuO and LiBiO2 additions, the d33 and sintering temperature of conventional lead-based ceramics have been listed in Figure 6. As is seen, the PHT-PNN ceramics with various sintering aids possess excellent piezoelectric properties while sintered at 950, 1000 and 1050∘C. However, a large amount of precious Hf elements were contained in the PHT-PNN ceramics, seriously limiting their industrial applications. Here-into, the d33 of the ceramic achieved in this work shows the high value among the low-temperature sintering piezoceramics ever reported in the literature.

Figure 6 Piezoelectric properties of lead-based ceramics fabricated by low-temperature sintering [21, 22, 23].
Figure 6

Piezoelectric properties of lead-based ceramics fabricated by low-temperature sintering [21, 22, 23].

5 Conclusions

  1. Aseries of 0.3 Pb(Ni1/3Nb2/3)O3-0.7 Pb(Zr0.41Ti0.59)O3 + x wt.% CuO + y wt.% LiBiO2 piezoelectric ceramics with a pure perovskite structure were successfully achieved by the low-temperature solid-state reaction.

  2. The CuO and LiBiO2 are suitable sintering aids for improving effectively the electric performance of piezoelectric ceramics. The rhombohedral and tetragonal phase are coexisted in PNN-PZT sample when x = 0.2 and y = 1, in which showed outstanding electric properties in the MPB. The d33, kp, єr, tan δ and Tc are 608 pC·N−1, 0.65, 3843, 2.19% and 191.6∘C respectively.

  3. The diffusion phase transition and the dielectric relaxation characteristics associated with Curie temperature can be found in this series, especially when x = 0.2 and y = 2, the sample shows the lowest Tc, the maximum of diffusion phase transition and dielectric relaxation behavior.

Acknowledgement

This paper is supported by Industrial research project of Guizhou Provincial Science and Technology Department of China (NO.(2015) 3005).

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Received: 2020-06-09
Accepted: 2020-09-22
Published Online: 2020-11-07

© 2020 J. Zhang et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/secm-2020-0039
Schlagwörter für diesen Artikel
piezoelectric ceramics; low-temperature sintering; electric properties; dielectric relaxation
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  3. Al3Ti/ADC12 Composite Synthesized by Ultrasonic Chemistry in Situ Reaction
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  5. The effect of carbon nanotubes on the mechanical and damping properties of macro-defect-free cements
  6. Toughening Mechanism of the Bone — Enlightenment from the Microstructure of Goat Tibia
  7. Characterization of PVC/MWCNTs Nanocomposite: Solvent Blend
  8. Study on Macroscopic and Mesoscopic Mechanical Behavior of CSG based on Inversion of Mesoscopic Material Parameters
  9. Bearing properties and influence laws of concrete-filled steel tubular arches for underground mining roadway support
  10. Comparing Test Methods for the Intra-ply Shear Properties of Uncured Prepreg Tapes
  11. Investigation of Microstructural, Mechanical and Corrosion Properties of AA7010-TiB2 in-situ Metal Matrix Composite
  12. A Comparative Study of Structural Changes in Conventional and Unconventional Machining and Mechanical Properties Evaluation of Polypropylene Based Self Reinforced Composites
  13. Research on Influence mechanism of composite interlaminar shear strength under normal stress
  14. Mechanical properties of geopolymer foam at high temperature
  15. Synthesis and mechanical properties of nano-Sb2O3/BPS-PP composites
  16. Multiscale acoustic emission of C/SiC mini-composites and damage identification using pattern recognition
  17. Modifying mechanical properties of Shanghai clayey soil with construction waste and pulverized lime
  18. Relationship between Al2O3 Content and Wear Behavior of Al+2% Graphite Matrix Composites
  19. Static mechanical properties and mechanism of C200 ultra-high performance concrete (UHPC) containing coarse aggregates
  20. A Parametric Study on the Elliptical hole Effects of Laminate Composite Plates under Thermal Buckling Load
  21. Morphology and crystallization kinetics of Rubber-modified Nylon 6 Prepared by Anionic In-situ Polymerization
  22. Effects of Elliptical Hole on the Correlation of Natural Frequency with Buckling Load of Basalt Laminates Composite Plates
  23. Effect of interphase parameters on elastic modulus prediction for cellulose nanocrystal fiber reinforced polymer composite
  24. Mixed Matrix Membranes prepared from polysulfone and Linde Type A zeolite
  25. Fabrication and low-velocity impact response of pyramidal lattice stitched foam sandwich composites
  26. Design and static testing of wing structure of a composite four-seater electric aircraft
  27. CSG Elastic Modulus Model Prediction Considering Meso-components and its Effect
  28. Optimization of spinning parameters of 20/316L bimetal composite tube based on orthogonal test
  29. Chloride-induced corrosion behavior of reinforced cement mortar with MWCNTs
  30. Statistical Law and Predictive Analysis of Compressive Strength of Cemented Sand and Gravel
  31. Young’s modulus and Poisson’s ratio of the deformable cement adhesives
  32. Reverse localization on composite laminates using attenuated strain wave
  33. Impact of reinforcement on shrinkage in the concrete floors of a residential building
  34. Novel multi-zone self-heated composites tool for out-of-autoclave aerospace components manufacturing
  35. Effect of notch on static and fatigue properties of T800 fabric reinforced composites
  36. Electrochemical Discharge Grinding of Metal Matrix Composites Using Shaped Abrasive Tools Formed by Sintered Bronze/diamond
  37. Fabrication and performance of PNN-PZT piezoelectric ceramics obtained by low-temperature sintering
  38. The extension of thixotropy of cement paste under vibration: a shear-vibration equivalent theory
  39. Conventional and unconventional materials used in the production of brake pads – review
  40. Inverse Analysis of Concrete Meso-constitutive Model Parameters Considering Aggregate Size Effect
  41. Finite element model of laminate construction element with multi-phase microstructure
  42. Effect of Cooling Rate and Austenite Deformation on Hardness and Microstructure of 960MPa High Strength Steel
  43. Study on microcrystalline cellulose/chitosan blend foam gel material
  44. Investigating the influence of multi-walled carbon nanotubes on the mechanical and damping properties of ultra-high performance concrete
  45. Preparation and properties of metal textured polypropylene composites with low odor and low VOC
  46. Calculation Model for the Mixing Amount of Internal Curing Materials in High-strength Concrete based on Modified MULTIMOORA
  47. Electric degradation in PZT piezoelectric ceramics under a DC bias
  48. Cushioning energy absorption of regular polygonal paper corrugation tubes under axial drop impact
  49. Erratum
  50. Study on Macroscopic and Mesoscopic Mechanical Behavior of CSG based on Inversion of Mesoscopic Material Parameters
  51. Effect of interphase parameters on elastic modulus prediction for cellulose nanocrystal fiber reinforced polymer composite
  52. Statistical Law and Predictive Analysis of Compressive Strength of Cemented Sand and Gravel
  53. Retraction
  54. Assessment of nano-TiO2 and class F fly ash effects on flexural fracture and microstructure of binary blended concrete
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Heruntergeladen am 15.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/secm-2020-0039/html
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