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Dielectric Characterization of Microwave Sintered Lead Zirconate Titanate Ceramics

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Dielectric Characterization of Microwave Sintered Lead Zirconate Titanate Ceramics Ceramics International 42 (2016) 14423–14430 Contents lists available at ScienceDirect Ceramics International journal homepage: www.elsevier.com/locate/ceramint Dielectric characterization of microwave sintered lead zirconate titanate ceramics Mayra D. Gonçalves a, Flavio L. Souza b, Elson Longo c, Edson R. Leite a, Emerson R. Camargo a,n a LIEC-Department of Chemistry, UFSCar - Federal University of São Carlos. São Carlos, SP, Brazil b UFABC - Federal University of ABC. Santo André, SP, Brazil c Institute of Chemistry UNESP, São Paulo State University. Araraquara, SP, Brazil article info abstract Article history: Highly reactive lead zirconate titanate powders (PZT) with different compositions were successfully Received 10 March 2016 synthesized by the oxidant-peroxo method (OPM) and used to prepare dense ceramic samples with Received in revised form composition near to the morphotropic phase boundary (MPB) sintered at 1000 °C for 2 h using a tubular 7 May 2016 conventional oven and a commercial microwave system. Crystalline phases were identified in the Accepted 6 June 2016 powder and ceramic samples by X-ray powder diffraction and FT-Raman spectroscopy at room tem- Available online 8 June 2016 perature. The fractured surface of the ceramic sample showed a high degree of densification with fairly Keywords: uniform grain sizes. Dielectric constants measured in the range from 30 to 500 °C at different frequencies PZT (1, 10 and 100 kHz) indicated a normal ferroelectric behavior regardless of the sintering method. Samples Chemical synthesis sintered by a microwave radiation (MW) method and composition near to the MPB region showed a Dielectric response maximum dielectric constant of 17.911 and an anomalous high Curie temperature of 465 °C. Sintering & Ceramics 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved. 1. Introduction This reaction results in an amorphous and reactive precipitate free of any common contaminants found in materials synthesized by Polycrystalline lead zirconate titanate (PZT) has attracted con- other routes that use organic compounds to stabilize cations in siderable attention due to its technological importance and ver- solution [6–8]. Usually, residual carbon can be eliminated only satile properties, particularly in the so-called morphotropic phase after annealing at high temperatures, however it completely boundary (MPB) region that occurs at nearly equal concentrations modifies the final properties and destroy the quality of powders of Ti4 þ and Zr4 þ . In this region, piezoelectric coefficients and di- synthesized by wet-chemical routes [9,10]. electric constants exhibit an anomalously sharp maximum during Although powders synthesized by the OPM route show evident the transition from Ti-rich tetragonal to Zr-rich rhombohedral advantages regarding purity, reactivity, particle size and size dis- fi fi phases [1]. The traditional route to obtain PZT involves reactions tribution, many of the nal properties of ne ceramics are de- between metal oxides or carbonates at high temperatures [2,3]. termined by the sintering procedure. Conventionally, PZT ceramics ° However, this technique suffers from a number of uncertainties require high temperatures exceeding 1250 C, which is undesir- and drawbacks that result in severe stoichiometry deviations. The able due to lead volatilization and a consequent loss in the com- presence of impurities in raw materials, the lack of homogeneity position that adversely affects the piezoelectric properties [11]. There has been a growing interest in the heating and sintering of due to poor mixing as well as a wide particle size distribution are ceramics by microwave radiation [12]. Since the first study de- major problems that led to the development of several alternative monstrating that PZT can be successfully prepared by the OPM techniques to synthesize ceramic powders [4]. The oxidant per- route [13], efforts have been directed toward obtaining dense oxide method (OPM) is one of the most interesting wet-chemical ceramics [14]. Apart from the extensive data available for PZT, little routes for the synthesis of lead or bismuth based materials [5]. is known about the use of microwaves. Recently, Raju and Reddy This route was named to as the oxidant peroxo method (OPM) and [15] reported the influence of microwave sintering on the struc- is based in the fundamental oxy-reduction reaction between lead tural and dielectric properties of lead zirconate titanate using very (II) ions and several water-soluble titanium peroxo complexes. reactive powders synthesized by the citrate method with a com- position around the MPB. Ramana et al. [16] compared microwave n Corresponding author. sintering with the conventional method using PZT powders syn- E-mail address: [email protected] (E.R. Camargo). thesized by the solid state reaction and concluded that microwave http://dx.doi.org/10.1016/j.ceramint.2016.06.035 0272-8842/& 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved. 14424 M.D. Gonçalves et al. / Ceramics International 42 (2016) 14423–14430 radiation can improve the densification at lower temperatures and same composition of the sample. The relative densities of sintered can also reduce the soaking time. In this process, heat is generated samples were measured using the Archimedes method. internally within the material instead of originating from external sources and is responsible for a unique microstructure and uni- 2.2. Characterization formity [17]. It should be noted that all these studies indicated that microwave sintering is a promising technique to obtain highly Amorphous precursors (10 mg) were analyzed by differential dense ceramics with superior dielectric behavior. scanning calorimetry (Netzsch DSC 204 Phoenix) in the range from In this study, we are presenting the synthesis of lead zirconate À100 to 550 °C at heating rate of 10 °C minÀ1 under a nitrogen titanate powders by the OPM route and the electrical character- atmosphere. The amorphous precursor, heat-treated powders and ization of dense ceramic bodies with composition near to the MPB all sintered samples were characterized at room temperature by region sintered by conventional and microwave processing, which Fourier transform Raman spectroscopy (FT-Raman, Bruker RFS resulted in ceramics with a maximum dielectric constant of 17.911 100/S) using the 1064 nm line of a yttrium aluminum garnet laser. and an anomalous high Curie temperature of 465 °C. These samples were also characterized by X-ray diffraction (XRD) using Cu Kα radiation (Rigaku D/MAX 200 with a rotary anode operating at 150 kV and 40 mA) in the 2θ range from 5° to 75° 2. Experimental with a step scan of 0.02°. The specific area of PZT powder heat- treated at 700 °C for 2 h was determined by BET isotherms using a 2.1. Synthesis and sintering Micromeritics ASAP 2000. The powder morphology was verified by transmission electron microscopy (TEM, Philips CM200), and All chemical reagents were used as received. Three nominal the cleaved sintered ceramics were characterized by high-resolu- compositions of Pb(Zr1ÀxTix)O3 (x¼0.20, 0.48 and 0.80, with tion field emission scanning electron microscopy (FE-SEM, Zeiss samples referred to as PZTX where “X” indicates the percentage of Supra 35 at 2 kV). The fractured surface composition was de- titanium) were prepared by the OPM route [5]. In a typical pro- termined by energy dispersive X-ray (EDX) spectroscopy (FEI XL30 cedure, 1 g (0.02 mol) of titanium metal powder (99.7%, Aldrich, FEG with an Oxford Instruments – Link ISIS 300 detector). For the Germany) was added into a mixture of 80 mL of hydrogen per- electrical measurements, gold contacts were sputtered on two oxide (analytical grade, Synth, Brazil) and 20 mL of aqueous am- opposite faces of the disks, and the dielectric constant (ε’) of the monia solution (analytical grade, Synth, Brazil). This solution was sintered samples was measured in the temperature range from 30 left in an ice-water bath for approximately 5 h, resulting in a to 500 °C using a Keithley 3330 (LCZ) meter at different fre- yellow transparent aqueous solution of soluble peroxytitanate quencies (1, 10, and 100 kHz). Two different heating rates were À ° À1 ° À1 [Ti(OH)3O2] ions. Zirconyl (IV) nitrate hydrate (ZrO(NO3)2 Á H2O, evaluated (1 and 5 C min ) and the 1 C min was choose to 99.99%, Aldrich, Germany) was previously submitted to gravi- carry out to measure the dielectric constant. In order to guarantee metric analysis by heat treatment at 900 °C for 2 h to estimate the the furnace temperature stability, each value of the dielectric exact molar quantity of zirconium per gram. The ZrO(NO3)2 Á H2O constant was collected only after leaving the sample for 30 min in was weighed and added into 100 mL of deionized water and lead each temperature. nitrate (99.9%, Aldrich, Germany) was added to complete the de- sired stoichiometric molar ratio. Finally, the solution of zirconium and lead nitrates was slowly dripped into the peroxytitanate so- 3. Results and discussion lution under stirring, resulting in a vigorous evolution of gas. The system lost its yellow color and an orange precipitate formed Although PZT is widely investigated, there are only a few stu- immediately exothermically. This precipitate was filtered and dies about PZT powders synthesized by the OPM route [5,13]. washed with diluted ammonia to eliminate nitrate ions. The wa- Despite this fact, it is well known that the amorphous precipitate shed amorphous precipitate was dried at 50 °C for 5 h and ground is rich is peroxide groups that release a large amount of oxygen gas using a mortar. Amounts of 0.20 g of the amorphous powder were during their exothermic decomposition [5–8,13,14,18]. For this calcined between 400 and 900 °C for 2 h using a heating rate of reason, sintered ceramics prepared directly from the amorphous À 10 °C min 1 in closed alumina boats.
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