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Abstract

The Focused Ion Beam (FIB) technique was applied for cross section preparation of the oxidized alloy for Transmission Electron Microscopy (TEM) study. Prior to preparation, the specimens of Fe-20Cr-5Al alloy sheet were oxidized in air at 1200 oC for 2 minutes, 10 minutes, 2 hours, and 100 hours. The microstructure and elemental composition of the samples were characterized using TEM equipped with an Energy Dispersive X-Ray Spectroscopy (EDX). The Electron Energy Loss Spectroscopy (EELS) was used to determine of the light elements. The TEM investigation reveals remarkable microstructure evolution of the specimens during oxidation which generally exhibit a typical multi-layer structure. The TEM images, however, can provide detailed description about the phases occur after oxidation such as the Tungsten (W) and the Gallium (Ga) layers on top of the samples obviously formed during FIB preparation, the formation of Al2O3 and Cr2O3 layer, MgAl2O4 spinel, porosity, Zr/Hf/Mg phases or clusters inside the oxide scale. Hence, the FIB technique has been proven to be reliable preparation technique for microstructural and elemental studies of Fe-20Cr-5Al alloy using TEM.

Bahasa Abstract

Karakterisasi TEM pada Paduan Fe-20Cr-5Al Oksidasi Temperatur Tinggi Menggunakan Teknik Preparasi FIB. Teknik Berkas Ion Terfokus atau Focused Ion Beam (FIB) diterapkan untuk persiapan melintang (cross section) aloi teroksidasi jenis Fe-20Cr-5Al untuk kajian Mikroskop Transmisi Elektron atau Transmission Electron Microscopy (TEM). Sebelum persiapan dilakukan, spesimen lembar aloi Fe-20Cr-5Al dioksidasi di udara pada suhu 1200 oC selama 2 menit, 10 menit, 2 jam, dan 100 jam. Struktur mikro dan komposisi elemen dari sampel tersebut dianalisis menggunakan TEM yang dilengkapi dengan Spektroskopi Sinar-X Energi Dispersif atau Energy Dispersive X-Ray Spectroscopy (EDX). Spektroskopi Kehilangan Energi Elektron atau Electron Energy Loss Spectroscopy (EELS) digunakan untuk menentukan elemen cahaya. Penggunaan TEM memperlihatkan evolusi struktur mikro yang luar biasa pada spesimen ketika oksidasi dilakukan, yang biasanya memperlihatkan struktur berlapis yang tipikal. Citra TEM memberikan deskripsi yang mendetail mengenai berbagai fase yang muncul setelah oksidasi, seperti lapisan Tungsten (W) dan Gallium (Ga) yang terbentuk di atas sampel selama masa persiapan FIB, pembentukan lapisan Al2O3 dan Cr2O3, spinel MgAl2O4, porositas, berbagai fase atau kelompok Zr/Hf/Mg di dalam skala oksida. Maka dari itu, teknik FIB telah terbukti sebagai teknik persiapan yang dapat diandalkan untuk meneliti struktur mikro dan elemen dari aloi Fe-20Cr-5Al dengan TEM.

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