Sains Malaysiana 47(3)(2018): 589–594

http://dx.doi.org/10.17576/jsm-2018-4703-20

 

Heat Treatment Effect on the Phase and Morphology of NiO-BCZY Prepared by an Evaporation and Decomposition of Solution and Suspension Method

(Kesan Rawatan Haba ke atas Fasa dan Morfologi NiO-BCZY yang Disediakan Melalui Kaedah Penyejatan dan Penguraian Larutan dan Mendakan)

 

ABDULLAH ABDUL SAMAT¹, SHAZANA MOHD SENARI², MAHENDRA RAO SOMALU¹,

ANDANASTUTI MUCHTAR^1,3, OSKAR HASDINOR HASSAN⁴ & NAFISAH OSMAN^2*

 

¹Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor Darul Ehsan, Malaysia

 

²Faculty of Applied Sciences, Universiti Teknologi MARA, 02600 Arau, Perlis Indera Kayangan, Malaysia

 

³Department of Mechanical and Materials Engineering, Faculty of Engineering and Built Environment, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor Darul Ehsan, Malaysia

 

⁴Department of Industrial Ceramics, Faculty of Art and Design, Universiti Teknologi MARA, 40450 Shah Alam, Selangor Darul Ehsan, Malaysia

 

Received: 10 April 2017/Accepted: 13 October 2017

 

ABSTRACT

A nitrate-based nickel salt was used to prepare NiO-BaCe_0.54Zr_0.36Y_0.1O_2.95 (NiO-BCZY) composite powders by an evaporation and decomposition of solution and suspension (EDSS) method. The prepared powders with different weight ratios of NiO to BCZY (NiO:BCZY) were denoted as S1 (50:50) and S2 (60:40). The powders were characterized using Thermogravimertic analyzer (TGA), X-ray diffractometer (XRD) and scanning electron microscope (SEM) equipped with energy dispersive X-ray (EDX) spectrometer. TGA results showed that the thermal decomposition of intermediate compounds in the dried powder (T = 150°C) completed at ~700°C. XRD analysis confirmed that the calcined powder (T = 1100°C) of S1 and S2 did not show any crystalline peaks related to BCZY compound as the peaks associated to impurity phases of BaCeO₃ and BaZrO₃ were appeared in their XRD patterns. The impurity phases along with NiO still remained in the S1 sample after it was calcined at 1400°C. As the calcination temperature increased, the particles size of S1 also increased and Zr elemental composition deviates from the nominal stoichiometric of the NiO-BCZY as proven by SEM/EDX analysis. The results indicate that the formation of homogenize NiO-BCZY composite prepared using EDSS method was not favored even after calcined at high temperature (T = 1400°C).

 

Keywords: Anode; composite; EDSS method; NiO-BCZY

 

ABSTRAK

Nikel berasaskan garam nitrat telah digunakan dalam penyediaan serbuk komposit NiO-BaCe_0.54Zr_0.36Y0.1O_2.95 (NiO-BCZY) melalui kaedah penyejatan dan penguraian larutan dan mendakan (EDSS). Serbuk yang terhasil dengan nisbah berat NiO kepada BCZY (NiO:BCZY) yang berbeza telah dilabelkan sebagai S1 (50:50) dan S2 (60:40). Serbuk tersebut telah dicirikan dengan menggunakan penganalisis termogravimetri (TGA), pembelauan sinar-X (XRD) dan mikroskop elektron pengimbas (SEM) yang dilengkapi dengan spektrometer sinar-X sebaran tenaga (EDX). Keputusan TGA menunjukkan penguraian terma sebatian pertengahan bagi serbuk yang dikeringkan (T = 150°C) telah lengkap pada suhu ~700°C. Analisis XRD mengesahkan serbuk S1 dan S2 yang telah dikalsinkan (T = 1100°C) tidak menunjukkan sebarang puncak fasa kristal sebatian BCZY disebabkan oleh kehadiran fasa bendasing BaCeO₃ and BaZrO₃ di dalam spektrum XRD. Kehadiran fasa bendasing ini dan juga NiO masih kekal di dalam serbuk S1 setelah dikalsin pada suhu 1400°C. Saiz partikel serbuk S1 bertambah apabila suhu pengkalsinan meningkat dan komposisi elemen Zr di dalam sampel menyimpang daripada stoikiometri sebenar NiO-BCZY seperti dibuktikan oleh analisis SEM/EDX. Keputusan daripada pencirian ini menunjukkan bahawa pembentukan fasa homogen komposit NiO-BCZY yang disediakan secara EDSS tidak dapat diperoleh walaupun selepas dikalsinkan pada suhu tinggi (T = 1400°C).

 

Kata kunci: Anod; kaedah EDSS; komposit; NiO-BCZY

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