Sains Malaysiana 43(9)(2014): 1373–1378

Characterization of Cerate-Zirconate Ceramics Powder Prepared by

Three Different Methods: A Comparative Study

(Pencirian Serat-Zirkonat Seramik Serbuk Disediakan oleh Tiga Kaedah yang Berbeza:

Suatu Kajian Perbandingan)

NAFISAH OSMAN¹*, NAJWA ‘ADNI IBARAHIM^1,2, MOHD AZLAN MOHD ISHAK¹ & OSKAR HASDINOR HASSAN³

¹Faculty of Applied Sciences, Universiti Teknologi MARA, 02600 Arau, Perlis

Malaysia

²Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam,

Selangor Darul Ehsan, Malaysia

³Faculty of Art and Design, Universiti Teknologi MARA, 40450 Shah Alam,

Selangor Darul Ehsan, Malaysia

Received: 15 May 2013/Accepted: 1 May 2014

ABSTRACT

Ceramics powder of BaCe_0.54Zr_0.36Y_0.1O_2.95 (BCZY) was synthesized using three different methods namely sol-gel (SG), supercritical fluid (SC) and supercritical fluid assisted sol-gel (SCSG). The respective prepared samples were denoted as S₁, S₂ and S₃. TG thermogram of the dried powders for all samples showed three stages of weight loss. Each stage was corroborated by one or two exothermic peaks as shown in DTG signal. Complete thermal decomposition for all the samples was almost accomplished at 1000°C for about 2 h. At calcination temperature of 1100°C, S1 showed a single-phase of perovskite-type oxides as proven by XRD result. Morphology of the calcined powders by SEM micrograph showed that S₁ is in spherical shape, S₂ is in cubic structure and S₃ has a mixture of spherical and rod-like structure. Therefore, as comparison, SG method gives better characteristics of cerate-zirconate ceramics powder compared to SC and SGSC.

Keywords: Cerate-zirconate ceramic; sol-gel; supercritical fluid; supercritical fluid assisted sol-gel

ABSTRAK

Serbuk seramik BaCe_0.54Zr_0.36Y_0.1O_2.95 (BCZY) telah disintesis menggunakan tiga kaedah yang berbeza iaitu sol-gel (SG), bendalir lampau genting (SC) dan bendalir lampau genting dibantu sol-gel (SGSC). Sampel masing-masing telah ditandakan sebagai S₁, S₂ dan S₃. Isyarat TG bagi semua serbuk sampel yang dikeringkan telah menunjukkan tiga peringkat kehilangan berat. Setiap peringkat kehilangan diiringi oleh satu atau dua puncak eksotermik seperti ditunjukkan oleh isyarat DTG. Penguraian terma yang lengkap untuk semua sampel didapati hampir sempurna pada suhu 1000°C selama 2 jam. Pada suhu pengkalsinan 1100°C, S1 menunjukkan satu fasa tunggal oksida perovksite seperti dibuktikan oleh analisis XRD. Morfologi serbuk yang dikalsinkan menggunakan mikrograf SEM mendedahkan S₁ adalah dalam bentuk sfera, S₂ berbentuk kubus dan S₃ adalah campuran bentuk sfera dan rod. Sebagai perbandingan, didapati kaedah SG memberi ciri serbuk seramik serat-zirkonat yang lebih baik daripada SC dan SGSC.

Kata kunci: Cecair genting lampau; cecair genting lampau membantu sol-gel; serat-zirkonat seramik; sol-gel

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*Corresponding author; email; fisha@perlis.uitm.edu.my