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 MUCHTAR1,3, OSKAR HASDINOR HASSAN4 & NAFISAH OSMAN2*

 

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-BaCe0.54Zr0.36Y0.1O2.95 (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-BaCe0.54Zr0.36Y0.1O2.95 (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

 

 

 

 

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