Pengaruh Konsentrasi Dopan Kalsium dan Sumber Kalsium Terhadap Struktur dan Kekerasan Ca-Zro2 Berbasis Pasir Zirkon

Setopratama, Andyan Rafi (2026) Pengaruh Konsentrasi Dopan Kalsium dan Sumber Kalsium Terhadap Struktur dan Kekerasan Ca-Zro2 Berbasis Pasir Zirkon. Masters thesis, Institut Teknologi Sepuluh Nopember.

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Abstract

Zirkonia (ZrO2) merupakan keramik biomedis yang berpotensi tinggi untuk gigi tiruan karena sifat mekanik dan biokompatibilitasnya. Penelitian ini bertujuan mengevaluasi dua hal utama yaitu pengaruh variasi konsentrasi dopan kalsium terhadap struktur kristal, densitas, kekerasan, dan morfologi keramik Ca-ZrO2, serta perbedaan antara sumber kalsium komersial dan cangkang telur ayam negeri terhadap pembentukan fasa, mikrostruktur, dan sifat mekanik yang dihasilkan. ZrO2 disintesis dari pasir alam zirkon lokal melalui metode fusi alkali–ko-presipitasi menghasilkan kemurnian 85,712 wt.%, kemudian didoping Ca, dikalsinasi pada 1100 °C, dan disinter pada 1400 °C. Karakterisasi dilakukan menggunakan XRD, spektroskopi Raman, SEM-EDX, kekerasan Vickers, densitas dan porositas. Penambahan Ca menginduksi pembentukan solid solution yang dikonfirmasi oleh pergeseran puncak difraksi, ekspansi sumbu c dari 5,100 menjadi 5,180 Å, dan penurunan microstrain dari 109,2 menjadi 53,1 × 10-4. Fraksi fasa tetragonal meningkat secara non-linier hingga 7,2 wt.% pada 1,0 mol% Ca, kemudian menurun akibat pengelompokan defek (defect clustering) dan segregasi batas butir. Densitas tertinggi dan porositas terendah dicapai pada 0,5% Ca komersial (4,473 g/cm3; porositas 19,15%) dengan kekerasan 140 HVN. Analisis SEM memperlihatkan morfologi butiran yang paling homogen dan pori paling kecil pada konsentrasi 0,5 mol% Ca, sementara konsentrasi lebih tinggi menghasilkan heterogenitas mikrostruktur yang berkorelasi langsung dengan peningkatan porositas. Sumber komersial dan cangkang telur menghasilkan karakteristik yang sebanding pada 0,5 mol%, dikonfirmasi oleh SEM-EDX yang menunjukkan morfologi butiran serupa dan kandungan Ca terdeteksi masing-masing 0,73 dan 0,97 wt.%. Nilai Ca EDX yang lebih tinggi pada sumber cangkang telur dikaitkan dengan kontribusi elemen jejak biogenik (Mg2+, Sr2+) dan kemungkinan tumpang tindih puncak energi pada detektor. Pada 1,0 mol%, cangkang telur menghasilkan fraksi ZrSiO4 pasca-sinter yang jauh lebih tinggi (60,3 vs. 23,1 wt.%) akibat elemen jejak biogenik bertindak sebagai mineralizer, yang juga terekam sebagai heterogenitas morfologi permukaan dan peningkatan porositas signifikan (32,79%) pada citra SEM. Cangkang telur ayam negeri terbukti efektif sebagai sumber kalsium biogenik pada konsentrasi 0,5 mol%, namun diperlukan optimasi parameter sintering untuk penelitian lebih lanjut.
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Zirconia (ZrO2) is a biomedical ceramic with high potential for dentures due to its mechanical properties and biocompatibility. This study aims to evaluate two main things, namely the effect of variations in calcium dopan concentration on the crystal structure, density, hardness, and morphology of Ca-ZrO2 ceramics, as well as the difference between commercial calcium sources and domestic chicken egg shells on phase formation, microstructure, and mechanical properties produced. ZrO2 is synthesized from local zircon natural sand by the alkali–co-precipitation fusion method resulting in a purity of 85.712 wt.%, then doped Ca, calcined at 1100 °C, and sintered at 1400 °C. Characterization was performed using XRD, Raman spectroscopy, SEM-EDX, Vickers hardness, density and porosity. The addition of Ca induced the formation of a solid solution confirmed by the shift of the diffraction peak, the expansion of the c-axis from 5,100 to 5,180 Å, and the decrease of the microstrain from 109.2 to 53.1 × 10-4. The tetragonal phase fraction increased non-linearly to 7.2 wt.% at 1.0 mol% Ca, then decreased due to defect clustering and grain boundary segregation. The highest density and lowest porosity were achieved at 0.5% commercial Ca (4.473 g/cm3; porosity 19.15%) with a hardness of 140 HVN. SEM analysis showed the most homogeneous granule morphology and the smallest pores at a concentration of 0.5 mol% Ca, while higher concentrations resulted in microstructural heterogeneity that was directly correlated with increased porosity. Commercial sources and eggshells yielded comparable characteristics at 0.5 mol%, confirmed by SEM-EDX which showed similar granule morphology and detected Ca content of 0.73 and 0.97 wt.%, respectively. Higher Ca EDX values at eggshell sources are associated with the contribution of biogenic trace elements (Mg2+, Sr2+) and the possible overlap of energy peaks in the detector. At 1.0 mol%, the eggshell produced a much higher post-sintered ZrSiO4 fraction (60.3 vs. 23.1 wt.%) due to biogenic trace elements acting as mineralizers, which were also recorded as surface morphological heterogeneity and significant increased porosity (32.79%) in SEM images. Chicken egg shells have been shown to be effective as a biogenic source of calcium at a concentration of 0.5 mol%, but optimization of sintering parameters is needed for further research.

Item Type:	Thesis (Masters)
Uncontrolled Keywords:	Cangkang telur, Dopan kalsium, Zirkonia, Calcium Doped, Eggshell, Zirconia
Subjects:	Q Science > QC Physics > QC100 Crystals. Q Science > QC Physics > QC111 Density and specific gravity T Technology > TN Mining engineering. Metallurgy > TN490 Zircon mines and mining T Technology > TS Manufactures > TS155 Production control. Production planning. Production management
Divisions:	Faculty of Industrial Technology and Systems Engineering (INDSYS) > Material & Metallurgical Engineering > 27101-(S2) Master Thesis
Depositing User:	Andyan Rafi Setopratama
Date Deposited:	24 Jul 2026 07:39
Last Modified:	24 Jul 2026 07:39
URI:	http://repository.its.ac.id/id/eprint/137232

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