Stabilized γ-BIMNVOX solid electrolyte: Ethylene glycol–citrate sol–gel synthesis, microwave-assisted calcination, and structural and electrical characterization

• Published in: Journal of alloys and compounds Vol. 581; pp. 79 - 85
• Main Authors: Al-Areqi, Niyazi A.S., Beg, Saba, Al-Alas, Ahlam, Hafeez, Shehla
• Format: Journal Article
• Language: English
• Published: Kidlington Elsevier B.V 25.12.2013; Elsevier
• Subjects: AC impedance spectroscopy; Calcination; Chemistry; Condensed matter: structure, mechanical and thermal properties; Electrical conductivity; Electrochemistry; Equations of state, phase equilibria, and phase transitions; Exact sciences and technology; General and physical chemistry; Physics; Properties of electrolytes: conductivity; Solid-solid transitions; Specific phase transitions; XRPD; γ-BIMEVOX; γ-BIMEVOX; Electrical conductivity; XRPD; AC impedance spectroscopy; Ethylene glycol; Scanning electron microscopy; Particle size; Electronic properties; Electrical properties; Crystallization; Solid electrolyte; Thermogravimetry; Citrate; Microwave; Differential thermal analysis; Microwave heating; X ray diffraction; Calcining; Powder pattern; Fine particle; Sol gel process; Xerogel
• ISSN: 0925-8388
• DOI: 10.1016/j.jallcom.2013.07.038

•γ-BIMNVOX was synthesized by ethylene glycol–citrate sol–gel route.•γ-BIMNVOX crystallizes by 25-min microwave-assisted calcination.•Smaller particle sizes for microwave calcined BIMNVOX samples.•Best oxide-ion performance for microwave calcined BIMNVOX samples. Samples of γ-BIMNVOX (Bi2V1−xMnxO5.5−x/2; 0.13⩽x⩽0.20) system were synthesized by an ethylene glycol–citrate sol–gel route. The resulting xerogels were then calcined by the microwave heating using a modified domestic microwave oven operated at 2.45GHz. Microwave-assisted calcination samples in comparison with other conventionally calcined samples were characterized in terms of phase crystallization, stabilization and particle size using simultaneous thermogravimetric–differential thermal analysis (TG–DTA), X-ray powder diffraction (XRPD) and scanning electron microscopy (SEM). The AC impedance spectroscopy was employed for electrical characterization. It was found that the microwave-assisted calcination route successfully produces better crystalline stabilized γ-BIMNVOX samples with appreciably small average particle sizes after only 25min of microwave heating. The electrical properties of microwave calcined γ-BIMNVOX system make it an advanced low-temperature solid electrolyte suitable for use in oxide-ion based electrochemical applications.