Analisis Stabilitas Fasa Dan Ukuran Kristal T-Zro2 Hasil Sintesis Dari Bahan Alam Dan Komersial Pada Temperatur Kalsinasi 800 Hingga 1100 oC

Ely, Sufilman (2022) Analisis Stabilitas Fasa Dan Ukuran Kristal T-Zro2 Hasil Sintesis Dari Bahan Alam Dan Komersial Pada Temperatur Kalsinasi 800 Hingga 1100 oC. Masters thesis, Institut Teknologi Sepuluh Nopember.

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Abstract

Penelitian ini dilakukan dengan tujuan mempelajari kestabilan fasa dan variasi ukuran kristal zirkonia tetragonal dari zirkonia bahan dasar pasir puya (ZP), zirkonia bahan dasar ZrCl4 komersial (ZK), dan ZK diberi dopan Ca berbahan dasar batu kapur alam (ZK-CA) yang dikalsinasi pada temperatur 800, 900, 1000 dan 1100 C selama 3 jam dan dengan variasi laju pemanasan. Pasir puya pada penelitian ini berasal dari Kereng Pangi, Kalimantan Tengah dan batu kapur alam berasal dari Rembang, Jawa Tengah. Serbuk ZrO2 amorf disintesis menggunakan metode alkali fusi dan kopresipitasi. Variasi laju pemanasan yang digunakan dalam penelitian ini adalah 5, 10, dan 15 oC/mnt dan variasi komposisi bahan dopan adalah 2,5 dan 5,0 at.%. Hasil karakterisasi X-ray Flourescence (XRF) menunjukkan bahwa serbuk zirkonia ZP memiliki impuritas alami, yaitu Si 1,7 wt.% dan Ti 2,9 wt.%, sedangkan serbuk ZK memiliki kemurnian hingga mencapai 99,6 wt.%. Hasil analisis data X-Ray Diffraction (XRD) serbuk ZP menunjukkan kestabilan fasa zirkonia tetragonal hingga temperatur 1000 oC dengan ukuran kristal minimum 10 nm dan maksimum 50 nm. Sedangkan hasil analisis data XRD serbuk ZK menunjukkan ketidakstabilan fasa zirkonia tetragonal dengan teridentifikasinya fasa monoklinik pada temperatur kalsinasi 800 oC. Penambahan dopan Ca pada serbuk ZK terbukti meningkatkan kestabilan fasa zirkonia tetragonal yang dikonfirmasi oleh hasil XRD yang menunjukkan fasa zirkonia tetragonal murni serbuk ZK-CA dapat stabil hingga temperatur kalsinasi 900 oC dengan ukuran minimum 27 nm dan maksimum 34 nm. Hasil analisis data XRD didukung oleh hasil pengujian Low Resolution-Transmission Electron Microscopy (LR-TEM) yang menunjukkan hasil yang serupa dengan XRD. Selanjutnya, hasil uji Particle Size Analyzer (PSA) dan Scanning Electron Microscope (SEM) menunjukkan bahwa kenaikan temperatur kalsinasi menyebabkan pertumbuhan partikel dan juga butir serbuk zirkonia. Berbeda dengan kenaikan temperatur, variasi laju pemanasan tidak berpengaruh besar terhadap stabilisasi fasa dan ukuran kristal. Hasil analisis XRD dan LR-TEM menunjukkan bahwa serbuk ZP memiliki kestabilan fasa yang lebih baik dan juga menghasilkan ukuran kristal yang lebih bervariasi.
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This research was conducted with the aim of studying the phase stability and the variation in crystallite size of tetragonal zirconia from puya sand (ZP), zirconia from commercial ZrCl4 (ZK), and ZK doped with Ca from natural limestone (ZK-CA) which were calcined at 800, 900, 1000 and 1100 oC for 3 hours and with heating rate variation. Puya sand in this study was from Kereng Pangi, Central Kalimantan and natural limestone was from Rembang, Central Java. Amorphous ZrO2 powder was synthesized using alkaline fusion and coprecipitation methods. The variation of the heating rate used in this study was 5, 10, and 15 oC/min and the variation of dopant composition was 2,5 and 5,0 at.%. The results of X-ray fluorescence (XRF) characterization showed that ZP zirconia powder had natural impurities, i.e. Si 1.7 wt.% and Ti 2.9 wt.%, while ZK powder had high purity reaching 99.6 wt.%. The results of the X-Ray Diffraction (XRD) data analysis of ZP powder showed the stability of the tetragonal zirconia phase up to a temperature of 1000 oC with a minimum crystal size of 10 nm and a maximum of 50 nm. On the other hand, the results of XRD data analysis of ZK powder showed the instability of the tetragonal zirconia phase with the identification of the monoclinic phase at a calcination temperature of 800 oC. The addition of Ca dopants to ZK powder was proven to increase the stability of the tetragonal zirconia phase which was confirmed by XRD results showing that the pure tetragonal zirconia phase of ZK-CA powder was stable up to a calcination temperature of 900 oC with a minimum size of 27 nm and a maximum of 34 nm. The results of the XRD data analysis were supported by the results of the Low Resolution-Transmission Electron Microscopy (LR-TEM) characterization which showed the same results with XRD results. The results of XRD and LR-TEM analysis showed that ZP powder had better phase stability and also produced more varied crystal sizes. Furthermore, the results of the Particle Size Analyzer (PSA) and Scanning Electron Microscope (SEM) showed that the increase in calcination temperature caused the growth of particles and grains of zirconia powder. On the other hand, variations in heating rate did not have a large effect on phase stabilization and crystallite size.

Item Type:	Thesis (Masters)
Uncontrolled Keywords:	zirkonia tetragonal (t-ZrO2), temperatur, laju pemanasan, dopan Ca, temperature, heating rate
Subjects:	T Technology > TA Engineering (General). Civil engineering (General) > TA418.16 Materials--Testing.
Divisions:	Faculty of Science and Data Analytics (SCIENTICS) > Physics > 45101-(S2) Master Thesis
Depositing User:	Mr. Marsudiyana -
Date Deposited:	12 Dec 2025 03:02
Last Modified:	12 Dec 2025 03:02
URI:	http://repository.its.ac.id/id/eprint/128945

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