Role of CA‐EDTA on the Synthesizing Process of Cerate‐Zirconate Ceramics Electrolyte

Abstract

The role of a combination between citric acid (CA) and ethylenediaminetetra acetic acid (EDTA) as chelating agents in preparation of BaCe0.54Zr0.36Y0.1O2.95powder by a modified sol-gel method is reported. The precursor solutions were prepared from metal nitrate salts (M+), chelating agents (C), and ethylene glycol (EG) at molar ratio of M+ : C : EG = 3 : 2 : 3. Chemical and phase transformation of samples during thermal decomposition were analyzed by thermogravimetric analysis (TGA) and Fourier transform infrared (FTIR) spectroscopy. TGA results show that the sample prepared by a combination of CA-EDTA exhibited the lowest thermal decomposition temperature,Ttdsince there was no significant weight loss after 750°C. After calcined at 1100°C, the carbonates residue remained in the samples as proven by FTIR results. It was found that the used combination of CA-EDTA acts as a better combustion reagent to increase the reaction rate and influence the thermal decomposition behaviour compared to a single citric acid and EDTA, respectively. Apparently, calcination temperatures above 1100°C are needed to produce a pure perovskitic BaCe0.54Zr0.36Y0.1O2.95.

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“…Meanwhile, the presence of secondary phases in S4 impurities of CeO 2 , (Ce,Zr)O 2 and BaCO 3 were observed in the XRD pattern. As reported in previous work, at this calcination temperature, the powder still consist remaining carbonate residue [7]. For the pellet sintered at 1300°C, the BaCO 3 impurity was decomposed and subsequently impeded a complete formation of BCZY.…”

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“…4) showed that the final weight loss occurred at a lower temperature for the EDTA-CA combination than for CA alone. It has previously been shown by Abdullah et al that in the sol-gel synthesis of BaCe0.54 Zr0.36 Y0.1 O2.95, gels prepared with an EDTA-CA combination exhibited lower thermal decomposition temperatures than gels prepared with EDTA or CA alone [38]. It was argued that the combination acted as a better combustion reagent to increase the reaction rate.…”

“…There are several sol-gel syntheses of perovskites reported in the literature in which EDTA and CA are used in combination, and many of them involve basic cations, such as Sr, Ba and La [38][39][40][41][42][43]. The interaction of EDTA and CA is clearly favourable for the formation of metal-organic precursor gels for these perovskite materials, although the mechanism is not completely understood.…”

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“…34,35 Hence this can explain why DTPA proved to be a better complexing agent than EDTA when not combined with CA. There are several sol-gel syntheses of perovskites reported in the literature in which EDTA and CA are used in combination, and many of them involve basic cations, such as Sr, Ba and La [37][38][39][40][41][42] . The interaction of EDTA and CA is clearly favourable for the formation of metal-organic precursor gels for these perovskite materials, although the mechanism is not completely understood.…”

“…It has previously been shown by Abdullah et al that in the sol-gel synthesis of BaCe0.54 Zr0.36 Y0.1 O2.95, gels prepared with an EDTA-CA combination exhibited lower thermal decomposition temperatures than gels prepared with EDTA or CA alone. 37 It was argued that the combination acted as a better combustion reagent to increase the reaction rate. As in our synthesis, Abdullah et al did not observe any weight loss by TGA after 750 °C, but 1100 °C was necessary to obtain phase purity.…”