Method for Cross-sectional Transmission Electron Microscopy Specimen Preparation of Composite Materials Using a Dedicated Focused Ion Beam System

Yaguchi, Toshie; Kamino, Takeo; Ishitani, Tohru; Urao, Ryoichi

doi:10.1017/s1431927699000203

Cited by 31 publications

(13 citation statements)

References 2 publications

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“…By adjusting the current density, the amount of material to be removed can be limited to the amount and area of the specimen required. The FIB mill procedure is described schematically in Figure 1 whereas the milling conditions are summarized in Table 2 [8,9]. Characterization.…”

Section: Methodsmentioning

confidence: 99%

Transmission Electron Microscopy Characterization of High-Temperatur Oxidation of Fe-20Cr-5Al Alloy Prepared by Focused Ion Beam Technique

Dani¹,

Untoro²,

Putra³

et al. 2015

MST

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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 o C 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 Al 2 O 3 and Cr 2 O 3 layer, MgAl 2 O 4 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. . Sebelum persiapan dilakukan, spesimen lembar aloi Fe-20Cr-5Al dioksidasi di udara pada suhu 1200 o C 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 Al 2 O 3 dan Cr 2 O 3, spinel MgAl 2 O 4 , 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. Abstrak

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Section: Methodsmentioning

confidence: 99%

Transmission Electron Microscopy Characterization of High-Temperatur Oxidation of Fe-20Cr-5Al Alloy Prepared by Focused Ion Beam Technique

Dani¹,

Untoro²,

Putra³

et al. 2015

MST

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“…These so-called liftout techniques were first proposed by Overwijk et al 4 and further developed to a routinely and reliably applicable technique for a broad materials range by Giannuzzi et al 5 Whereas the first attempts were based on an ex situ lift-out of the lamella using a micromanipulator under an optical microscope, techniques based on an in situ lift-out of the lamella are gaining increasing importance. 6 Specimens extracted by in situ lift-out can be shaped in a number of different and…”

Section: Specimen Preparation Techniquesmentioning

confidence: 99%

TEM Sample Preparation and FIB-Induced Damage

Mayer¹,

Giannuzzi²,

Kamino³

et al. 2007

MRS Bull.

Self Cite

793

486

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preparation can be applied to almost any material type-hard, soft, or combinations thereof. The number of materials for which successful TEM sample preparation with FIBs has been documented certainly reaches several hundred and spans from hard matter such as metals, ceramics, and composites to soft matter including polymers, biological materials, and even frozen liquids.The main disadvantage of FIBs, however, is caused by the nature of the milling process: the ion collisions initiating sputter removal can also lead to ion implantation and cause severe damage to the remaining bulk of the material. As the FIB lamellae method spreads to more advanced TEM techniques, various procedures have been developed to reduce or repair this damage.In this article, the major specimen preparation techniques are reviewed; the consequences of FIB-induced damage are discussed, along with strategies to reduce the damage; and an overview on applications in materials science and in related instrumental fields is presented. Specimen Preparation TechniquesSince the first-generation FIBs were mainly used as semiconductor tools, early attempts to prepare TEM specimens in an FIB also focused on semiconductor materials. The initial methods were based on mechanically polishing the sample down to an approximately 50-mm lamella and then using the FIB to cut two trenches, one from each side, leaving behind a thin electron-transparent lamella supported by bulk material on two opposite sides ( Figure 1). 2 Referring to the geometry seen in Figure 1, this method is frequently called the H-bar technique. This method was subsequently refined by employing a tripod polisher for the initial thinning of the thin slab, 3 which is particularly valuable in the case of complex semiconductor devices.In parallel, techniques were developed that make it possible to directly remove an electron-transparent lamella from a bulk specimen without mechanical polishing (see Figure 2). These so-called liftout techniques were first proposed by Overwijk et al. 4 and further developed to a routinely and reliably applicable technique for a broad materials range by Giannuzzi et al. 5 Whereas the first attempts were based on an ex situ lift-out of the lamella using a micromanipulator under an optical microscope, techniques based on an in situ lift-out of the lamella are gaining increasing importance. 6 Specimens extracted by in situ lift-out can be shaped in a number of different and 400 MRS BULLETIN • VOLUME 32 • MAY 2007 • www/mrs.org/bulletin AbstractOne of the most important applications of a focused ion beam (FIB) workstation is preparing samples for transmission electron microscope (TEM) investigation. Samples must be uniformly thin to enable the analyzing beam of electrons to penetrate. The FIB enables not only the preparation of large, uniformly thick, sitespecific samples, but also the fabrication of lamellae used for TEM samples from composite samples consisting of inorganic and organic materials with very different properties. This article gives an overview of the...

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“…12 The ion milling was conducted in three steps of decreasing beam current, using a procedure based on the lift-out method of transmission electron microscopy sample preparation. 11,20 An initial coarse milling step at a relatively high current of 14 nA was used to create a trench with a depth of 10 µm surrounding the region in which the sheet was fabricated. The trench was designed to allow subsequent characterization using x-ray nanodiffraction.…”

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confidence: 99%

Fabrication and convergent X-ray nanobeam diffraction characterization of submicron-thickness SrTiO3 crystalline sheets

et al. 2016

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The creation of thin SrTiO3 crystals from (001)-oriented SrTiO3 bulk single crystals using focused ion beam milling techniques yields sheets with submicron thickness and arbitrary orientation within the (001) plane. Synchrotron x-ray nanodiffraction rocking curve widths of these SrTiO3 sheets are less than 0.02°, less than a factor of two larger than bulk SrTiO3, making these crystals suitable substrates for epitaxial thin film growth. The change in the rocking curve width is sufficiently small that we deduce that dislocations are not introduced into the SrTiO3 sheets. Observed lattice distortions are consistent with a low concentration of point defects.

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Method for Cross-sectional Transmission Electron Microscopy Specimen Preparation of Composite Materials Using a Dedicated Focused Ion Beam System

Cited by 31 publications

References 2 publications

Transmission Electron Microscopy Characterization of High-Temperatur Oxidation of Fe-20Cr-5Al Alloy Prepared by Focused Ion Beam Technique

Transmission Electron Microscopy Characterization of High-Temperatur Oxidation of Fe-20Cr-5Al Alloy Prepared by Focused Ion Beam Technique

TEM Sample Preparation and FIB-Induced Damage

Fabrication and convergent X-ray nanobeam diffraction characterization of submicron-thickness SrTiO3 crystalline sheets

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