Cross-Sectional TEM Specimen Preparation for W/B4C Multilayer Sample Using FIB: A Recent Study

In thermal oxidation studies, the structure of the oxide-metal interface and the near-surface region is of great importance. A technique has been developed for constructing cross-sectional samples of oxidized aluminum alloys, which reveal these regions. The specimen preparation procedure is as follows: An ultra-sonic drill is used to cut a 3mm diameter disc from a 1.0mm thick sheet of the material. The disc is mounted on a brass block with low-melting wax, and a 1.0mm hole is drilled in the disc using a #60 drill bit. The drill is positioned so that the edge of the hole is tangent to the center of the disc (Fig. 1) . The disc is removed from the mount and cleaned with acetone to remove any traces of wax. To remove the cold-worked layer from the surface of the hole, the disc is placed in a standard sample holder for a Tenupol electropolisher so that the hole is in the center of the area to be polished.

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Ultramicrotomy as a Technique for Materials Specimen Preparation

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100135745 ◽

1990 ◽

Vol 48 (2) ◽

pp. 428-429

Author(s):

S.R. Glanvill

Keyword(s):

Materials Science ◽

Structural Information ◽

Specimen Preparation ◽

Preparation Technique ◽

Cross Sectional ◽

Surfaces And Interfaces ◽

Beam Analysis ◽

Flat Embedding ◽

20 Nm ◽

Sectional Analysis

This paper summarizes the application of ultramicrotomy as a specimen preparation technique for some of the Materials Science applications encountered over the past two years. Specimens 20 nm thick by hundreds of μm lateral dimension are readily prepared for electron beam analysis. Materials examined include metals, plastics, ceramics, superconductors, glassy carbons and semiconductors. We have obtain chemical and structural information from these materials using HRTEM, CBED, EDX and EELS analysis. This technique has enabled cross-sectional analysis of surfaces and interfaces of engineering materials and solid state electronic devices, as well as interdiffusion studies across adjacent layers.Samples are embedded in flat embedding moulds with Epon 812 epoxy resin / Methyl Nadic Anhydride mixture, using DY064 accelerator to promote the reaction. The embedded material is vacuum processed to remove trapped air bubbles, thereby improving the strength and sectioning qualities of the cured block. The resin mixture is cured at 60 °C for a period of 80 hr and left to equilibrate at room temperature.

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Cross-sectional TEM specimen preparation from magneto-optical disk by ultramicrotomy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100147028 ◽

1993 ◽

Vol 51 ◽

pp. 236-237

Author(s):

F. Shaapur ◽

M.J. Kim ◽

Seh Kwang Lee ◽

Soon Gwang Kim

Keyword(s):

System Development ◽

Thin Foil ◽

Specimen Preparation ◽

Material System ◽

Cross Sectional ◽

Protective Layers ◽

New Material ◽

Diamond Saw ◽

Original Production ◽

Thick Medium

TEM characterization and microanalysis of the recording media is crucial and complementary to new material system development as well as quality control applications. Due to the type of material generally used for supporting the medium, i.e., a polymer, conventional macro- and microthinning procedures for thin foil preparation are not applicable. Ultramicrotorny (UM) is a viable option and has been employed in previous similar studies. In this work UM has been used for preparation of XTEM samples from a magneto-optical (MO) recording medium in its original production format.The as-received material system consisted of a 4-layer, 2100 Å thick medium including a 300 Å TbFeCo layer enveloped by silicon nitride protective layers supported on a 1.2 mm thick × 135 mm (5.25 in.) diameter polycarbonate disk. Recording tracks had an approximate pitch of 1.6 μm separated by 800 Å deep peripheral grooves. Using a Buehler Isomet low-speed diamond saw, 1 mm wide and 20 mm long strips were cut out of the disk along the recording tracks.

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The Influence of Blade Type and Feeding Force during Resin Bonded Dentin Specimen Preparation on the Microtensile Bond Strength Test

Micromachines ◽

10.3390/mi12040450 ◽

2021 ◽

Vol 12 (4) ◽

pp. 450

Author(s):

Apinya Limvisitsakul ◽

Suppason Thitthaweerat ◽

Pisol Senawongse

Keyword(s):

Bond Strength ◽

Surface Integrity ◽

Strength Test ◽

Specimen Preparation ◽

Sectional Area ◽

Microtensile Bond Strength ◽

Cross Sectional ◽

Microtensile Testing ◽

Feeding Force ◽

Scanning Electron

This paper presents the effect of blade type and feeding force during resin-bonded dentin specimen preparation on the microtensile bond strength (μTBS) test. Forty resin-bonded flat middle dentin specimens were divided into four groups. The specimens of each group were sectioned according to type of blade and feeding force as follows: fine grit/20 N, fine grit/40 N, medium grit/20 N, and medium grit/40 N to obtain resin-dentin sticks with a cross-sectional area of 1.0 mm2. Four sticks from the center of each tooth were subjected to the μTBS test. Five remaining sticks of each group were selected for surface topography observation under a scanning electron microscope (SEM). As a result, the bond strength of the medium-grit group was higher than that of the fine-grit group (p < 0.001), whereas the feeding force had no influence on bond strength values (p = 0.648). From the SEM, sticks prepared with the fine-grit blade showed a smoother surface integrity and fewer defects on the specimen edges in comparison with the sticks prepared with the medium-grit blade. The grit type of the blade is one of the considerable factors that may affect the bond strength and the surface integrity of resin-dentin specimens for microtensile testing.

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Comparison of Focused Ion Beam and Conventional Techniques on Tem Specimen Preparation of Metal-Ceramic Interfaces

Microscopy and Microanalysis ◽

10.1017/s1431927600024429 ◽

1998 ◽

Vol 4 (S2) ◽

pp. 860-861 ◽

Cited By ~ 1

Author(s):

A. Ramirez de Arellano López ◽

W.-A. Chiou ◽

K. T. Faber

Keyword(s):

Focused Ion Beam ◽

Ceramic Coating ◽

Steel Substrate ◽

Ion Beam ◽

Specimen Preparation ◽

Inhomogeneous Materials ◽

Cross Sectional ◽

Fine Grain ◽

Basic Industry ◽

Coated Surface

The results of TEM analyses of materials are critically dependent on the quality of the sample prepared. Although numerous techniques have been developed in the last two decades, differential thinning of inhomogeneous materials remains a serious problem. Recently, focused ion beam (FIB) technique has been introduced for cross-sectional sample preparation for TEM and SEM.A novel system for depositing a fine-grain (∼ 200 nm) ceramic coating on a metal surface via a patent pending Small-Particle Plasma Spray (SPPS) technique has been developed at the Basic Industry Research Laboratory of Northwestern University. To understand the properties of the coated surface, the ceramic/metal interface and the microstructure of the ceramic coating must be investigated. This paper presents a comparison of the microstructure of an A12O3 coating on a mild steel substrate prepared using conventional and FEB techniques.

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Method for Cross-sectional Thin Specimen Preparation from a Specific Site Using a Combination of a Focused Ion Beam System and Intermediate Voltage Electron Microscope and Its Application to the Characterization of a Precipitate in a Steel

Microscopy and Microanalysis ◽

10.1007/s100050010065 ◽

2001 ◽

Vol 7 (3) ◽

pp. 287-291

Author(s):

Toshie Yaguchi ◽

Hiroaki Matsumoto ◽

Takeo Kamino ◽

Tohru Ishitani ◽

Ryoichi Urao

Keyword(s):

Electron Microscope ◽

Focused Ion Beam ◽

Ion Beam ◽

Specific Site ◽

Specimen Preparation ◽

Thin Specimen ◽

Cross Sectional ◽

Electron Detector ◽

Specimen Holder

AbstractIn this study, we discuss a method for cross-sectional thin specimen preparation from a specific site using a combination of a focused ion beam (FIB) system and an intermediate voltage transmission electron microscope (TEM). A FIB-TEM compatible specimen holder was newly developed for the method. The thinning of the specimen using the FIB system and the observation of inside structure of the ion milled area in a TEM to localize a specific site were alternately carried out. The TEM fitted with both scanning transmitted electron detector and secondary electron detector enabled us to localize the specific site in a halfway milled specimen with the positional accuracy of better than 0.1 µm. The method was applied to the characterization of a precipitate in a steel. A submicron large precipitate was thinned exactly at its center for the characterization by a high-resolution electron microscopy and an elemental mapping.

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A Method for Site Specific Characterization Using a Dedicated FIB System Combined With an Analyitical TEM

Microscopy and Microanalysis ◽

10.1017/s143192760001789x ◽

1999 ◽

Vol 5 (S2) ◽

pp. 914-915

Author(s):

T. Kamino ◽

T. Yaguchi ◽

H. Matsumoto ◽

H. Kobayashi ◽

H. Koike

Keyword(s):

Focused Ion Beam ◽

Ion Irradiation ◽

Ion Beam ◽

System Stability ◽

Specimen Preparation ◽

Thin Specimen ◽

Cross Sectional ◽

Site Specific ◽

Specimen Holder ◽

High Resolution Tem

A method for site specific characterization of the materials using a dedicated focused ion beam(FIB) system and an analytical transmission electron microscope (TEM) was developed. Needless to say, in TEM specimen preparation using FIB system, stability of a specimen is quite important. The specimen stage employed in the developed FIB system is the one designed for high resolution TEM, and the specimen drift rate of the stage is less than lnm/min. In addition, FIB-TEM compatible specimen holder which allows milling of a specimen with the FIB system and observation of the specimen with the TEM without re-loading was developed. To obtain thin specimen from the area to be characterized correctly, confirmation of the area before final milling is needed. However, observation of cross sectional view in a FIB system is recommended because it causes damage by Ga ion irradiation. To solve this problem, we used a STEM unit as a viewer of FIB milled specimen.

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Tem Specimen Preparation for Display Materials of Vacuum Fluorescent Displays

Microscopy and Microanalysis ◽

10.1017/s1431927600024478 ◽

1998 ◽

Vol 4 (S2) ◽

pp. 870-871

Author(s):

T. Dolukhanyan ◽

C. Sung ◽

S. Ahn ◽

J. Lee

Keyword(s):

Bulk Material ◽

Low Cost ◽

High Yield ◽

Specimen Preparation ◽

List Type ◽

Ion Milling ◽

Cross Sectional ◽

Preparation Methods ◽

Plan View ◽

Submicron Scale

Further development of Vacuum Fluorescent Displays (Fig.l) for low cost production and high yield requires investigation of all the components on a submicron scale at various processing stages.A variety of specimen preparation methods have been used for making different types of high quality cross-sectional and plan-view TEM specimens from:1.Initial phosphor materials - ZnCdS powders admixed with conducting powder of ln2O3;2.In2O3 mixed ZnCdS phosphor layers of ready-made working VFD;3.W - filament cathodes coated with (Ba,Sr,Ca) oxides.Rapid sharing of results.Group 1 specimens were made both by direct dispersion of phosphor powder particles on the carbon coated copper grid from acetone diluted powder suspension, and by preparation of cured bulk material from the powder using Gatan G-l epoxy, followed by cutting, grinding-dimpling and final ion milling in Gatan DuoMill 600 (Fig.2).

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