Malaysian Journal of Analytical Sciences Vol 19 No 6 (2015): 1284 - 1289

 

 

 

ANALYSIS OF THERMOGRAVIMETRIC (TG) AND INFRA-RED (FTIR) ON Dy SUBSTITUTION IN Bi(Pb)-2223 SUPERCONDUCTOR

 

(Analisis Termogravimetri (TG) dan Infra-Merah (FTIR) ke atas pemasukan Dy dalam Superkonduktor Bi(Pb)-2223)

 

Siti Hawa Jamil¹, Azhan Hashim²*, Syed Yusainee Syed Yahya¹, Azman Kasim², Nurul Hidayah Hasan¹,

Norazidah Abdul Wahab¹

 

¹Faculty of Applied Sciences,

Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

²Faculty of Applied Sciences,

Universiti Teknologi MARA Pahang, 26400 Jengka, Pahang, Malaysia

 

*Corresponding author: dazhan@pahang.uitm.edu.my

 

 

Received: 23 November 2014; Accepted: 3 September 2015

 

 

Abstract

In this paper, the results of the thermal and infra-red analysis of Dy substituted in Bi (Pb)-2223 superconductor have been studied by thermogravimetric (TG) and Fourier transform infrared (FTIR). The samples with nominal composition of Bi_1.6Pb_0.4Sr₂Ca_2-xDy_xCu₃O_y where x = 0.000, 0.025, 0.050, 0.100, and 0.200 were prepared by co-precipitation (COP) method using metal acetate as the starting salts. The mechanism of thermal analysis of the precursor powder for each stage (drying, precalcine, and calcine) were studied from 20 °C to 920 °C by 5 °C/min of heating rate. Interestingly, the thermal decomposition proceeds in the almost similar way regardless of the Dy substitution level with five major drops at the drying stage. Based on TG curves results, the temperature range from 840 °C to 850 °C can be suggested as an optimum calcination and sintering temperature. The majority of decomposition step which related to the loss of water from oxalate was in the range of 100 °C to 200 °C while the formation of precipitation into Bi₂O₃, PbO, SrCO₃, CaCO₃, CuO, and Dy₂O₃ were in the range of 210 °C to 360 °C. From the FTIR result, all the precursor powders qualitatively showed four main regions and the existence of –OH group can increase the diffusion rate between metals during the synthesis process.

 

Keywords: dy-substitution, BSCCO, superconductor, FTIR, thermogravimetric analysis

 

Abstrak

Dalam laporan ini, keputusan analisa terma dan infra-merah terhadap pemasukan Dy di dalam superkonduktor Bi (Pb)-2223 telah dikaji melalui termogravimetri dan transformasi fourier infra-merah (FTIR). Semua sampel dengan komposisi nominal Bi_1.6Pb_0.4Sr₂Ca_2-xDy_xCu₃O_y dimana x = 0.000, 0.025, 0.050, 0.100 dan 0.200 telah disediakan melalui kaedah ko-pemendakan (COP) dengan menggunakan logam asetat sebagai garam pemula. Mekanisma analis terma terhadap serbuk pelopor untuk setiap peringkat (pengeringan, pra-pengkalsinan dan pengkalsinan) telah dikaji dari suhu 20 °C hingga 920 °C dengan kadar pemanasan 5°C/min. Menariknya, penguraian terma berlaku agak sama tanpa menghiraukan aras pemasukan Dy iaitu dengan lima jatuhan pada peringkat pengeringan. Berdasarkan kepada keputusan keluk TG, dicadangkan bahawa julat suhu dari 840 °C hingga 850 °C  merupakan suhu pengkalsinan dan suhu sinteran optimum. Majoriti langkah penguraian yang berhubungkait dengan kehilangan air dari oksalat, berlaku dalam julat 210 °C hingga 360 °C manakala pembentukan pemendakan dalam Bi₂O₃, PbO, SrCO₃, CaCO₃, CuO, dan Dy₂O₃ adalah dalam julat 210 °C hingga 360 °C. Dari keputusan FTIR, semua serbuk pelopor secara kualitatifnya menunjukkan empat daerah utama dan keujudan kumpulan –OH boleh meningkatkan kadar peresapan antara logam semasa proses sintesis.

 

Kata kunci: pemasukan Dy, BSCCO, superkonduktor, FTIR, analisis termogravimetri

 

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