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

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.

Prospecting for gold in a VG STEM

1992 ◽  
Vol 50 (1) ◽  
pp. 412-413
Author(s):  
G. L Shoemaker ◽  
W. M. Sherman ◽  
R. H. Duff ◽  
D. R. Rothbard
Keyword(s):  
Iron Oxide ◽  
Thin Foil ◽  
Dark Field ◽  
Skeletal Structure ◽  
Specimen Preparation ◽  
Iron Pyrite ◽  
The Matrix ◽  
Annular Dark Field ◽  
Electron Image ◽  
Diamond Saw

A calcined pyritic gold ore concentrate was examined using both ion–milled and ultramicrotomed samples to determine the distribution of gold and the porosity of the matrix supporting the gold. Examinations of the same specimen prepared by different techniques yielded complementary information about the overall characteristics of the material.Figure 1 is a secondary electron image (SEI) of a piece of roasted pyritic ore. The particles are highly porous with morphology suggesting that the iron pyrite (FeS2) particles virtually exploded when labile sulfur was released during oxidative calcination. The particles produced by this process are not large enough to permit ordinary solid specimen preparation techniques. Therefore, a compacted bar of material was made by compressing the powder with a binder to form a disk which was subsequently impregnated with epoxy in a PARR bomb under isostatic pressure of a few thousand psi. From this dense material two types of specimen were prepared, one by diamond knife ultramicrotomy and the other by standard thin foil techniques. For the latter, the sample was sliced with a diamond saw, core–drilled into 3mm disks, polished to about 100μm, dimple ground, and Argon ion milled to perforation. This yielded specimens which show the porosity and connectivity of the iron oxide frameworks formed during calcination. Figure 2 is a 10,000X annular dark field (ADF) image of an ion–milled particle taken with a VG HB501 STEM. The channel structures evident in this image are easily related to the SEI image in Figure 1. Figure 3 is a 200,000X ADF image which illustrates the connectivity of individual iron oxide crystallites that form the skeletal structure. This sample was electron transparent only near the central perforation and did not have a large usable area. Also, the outer surfaces ot the particles may have been milled away during specimen preparation and therefore it is not easy to determine where the remaining structures were located in the original particles.

Development Process for Custom Three-Dimensional Printing (3DP) Material Systems

2010 ◽  
Vol 132 (1) ◽  
Author(s):  
Ben R. Utela ◽  
Duane Storti ◽  
Rhonda L. Anderson ◽  
Mark Ganter
Keyword(s):  
System Development ◽  
Three Dimensional ◽  
Research Problem ◽  
Processing Parameters ◽  
Clear Understanding ◽  
Material System ◽  
Three Dimensional Printing ◽  
Dense Ceramic ◽  
New Material ◽  
Dimensional Printing

The development of a new material system for three-dimensional printing (3DP) can be difficult without experience in the field, since the flexibility of the 3DP process implies a large number of material and processing parameters. This paper presents a detailed explanation of the steps involved in developing specific implementations of 3DP, along with tools and insight for each step. This material system development procedure should provide a clear understanding of the 3DP process steps and development decisions to help the user take advantage of the considerable flexibility of 3DP and expedite a new system development. The paper concludes with a demonstration of how the guidance provided is applied in the development of fully dense ceramic dental copings; a research problem uniquely suited to the flexibility of 3DP.

Preparation of cross-sectional samples for near-surface TEM studies

1987 ◽  
Vol 45 ◽  
pp. 380-381
Author(s):  
R.C. Dickenson ◽  
K.R. Lawless
Keyword(s):  
Standard Sample ◽  
Surface Region ◽  
Specimen Preparation ◽  
Thick Sheet ◽  
Drill Bit ◽  
Sample Holder ◽  
Metal Interface ◽  
Cross Sectional ◽  
Near Surface ◽  
Cold Worked

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.

Ultramicrotomy as a Technique for Materials Specimen Preparation

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.

Ion thinning of integrated circuit transverse specimens for transmission electron microscopy

1992 ◽  
Vol 50 (2) ◽  
pp. 1426-1427
Author(s):  
F. Shaapur
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Integrated Circuit ◽  
Substrate Surface ◽  
Homogeneous Material ◽  
Material System ◽  
Ion Milling ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Motion Profile

Non-uniform ion-thinning of heterogenous material structures has constituted a fundamental difficulty in preparation of specimens for transmission electron microscopy (TEM). A variety of corrective procedures have been developed and reported for reducing or eliminating the effect. Some of these techniques are applicable to any non-homogeneous material system and others only to unidirectionalfy heterogeneous samples. Recently, a procedure of the latter type has been developed which is mainly based on a new motion profile for the specimen rotation during ion-milling. This motion profile consists of reversing partial revolutions (RPR) within a fixed sector which is centered around a direction perpendicular to the specimen heterogeneity axis. The ion-milling results obtained through this technique, as studied on a number of thin film cross-sectional TEM (XTEM) specimens, have proved to be superior to those produced via other procedures.XTEM specimens from integrated circuit (IC) devices essentially form a complex unidirectional nonhomogeneous structure. The presence of a variety of mostly lateral features at different levels along the substrate surface (consisting of conductors, semiconductors, and insulators) generally cause non-uniform results if ion-thinned conventionally.

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

Micromachines ◽  
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.

scholarly journals Structural and compositional analysis of (InGa)(AsSb)/GaAs/GaP Stranski–Krastanov quantum dots

2021 ◽  
Vol 10 (1) ◽  
Author(s):  
Raja S. R. Gajjela ◽  
Arthur L. Hendriks ◽  
James O. Douglas ◽  
Elisa M. Sala ◽  
Petr Steindl ◽  
...  
Keyword(s):  
Quantum Dots ◽  
Flash Memory ◽  
Compositional Analysis ◽  
Structural Data ◽  
Scanning Tunneling ◽  
Valuable Insight ◽  
Material System ◽  
Tunneling Microscopy ◽  
Cross Sectional ◽  
Fe Simulations

AbstractWe investigated metal-organic vapor phase epitaxy grown (InGa)(AsSb)/GaAs/GaP Stranski–Krastanov quantum dots (QDs) with potential applications in QD-Flash memories by cross-sectional scanning tunneling microscopy (X-STM) and atom probe tomography (APT). The combination of X-STM and APT is a very powerful approach to study semiconductor heterostructures with atomic resolution, which provides detailed structural and compositional information on the system. The rather small QDs are found to be of truncated pyramid shape with a very small top facet and occur in our sample with a very high density of ∼4 × 1011 cm−2. APT experiments revealed that the QDs are GaAs rich with smaller amounts of In and Sb. Finite element (FE) simulations are performed using structural data from X-STM to calculate the lattice constant and the outward relaxation of the cleaved surface. The composition of the QDs is estimated by combining the results from X-STM and the FE simulations, yielding ∼InxGa1 − xAs1 − ySby, where x = 0.25–0.30 and y = 0.10–0.15. Noticeably, the reported composition is in good agreement with the experimental results obtained by APT, previous optical, electrical, and theoretical analysis carried out on this material system. This confirms that the InGaSb and GaAs layers involved in the QD formation have strongly intermixed. A detailed analysis of the QD capping layer shows the segregation of Sb and In from the QD layer, where both APT and X-STM show that the Sb mainly resides outside the QDs proving that Sb has mainly acted as a surfactant during the dot formation. Our structural and compositional analysis provides a valuable insight into this novel QD system and a path for further growth optimization to improve the storage time of the QD-Flash memory devices.

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

1998 ◽  
Vol 4 (S2) ◽  
pp. 860-861 ◽  
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.

Attribute Based Selection of Thermoplastic Resin for Vacuum Infusion Process

2011 ◽  
Vol 1 (3) ◽  
pp. 31-52 ◽  
Author(s):  
R. T. Durai Prabhakaran ◽  
Aage Lystrup ◽  
Tom Løgstrup Andersen
Keyword(s):  
Material System ◽  
Mathematical Tool ◽  
Thermoplastic Resin ◽  
Thermoplastic Polymers ◽  
Vacuum Infusion ◽  
Thermosetting Polymers ◽  
Current Scenario ◽  
New Material ◽  
Selection Of ◽  
Vacuum Infusion Process

The composite industry looks toward a new material system (resins) based on thermoplastic polymers for the vacuum infusion process, similar to the infusion process using thermosetting polymers. A large number of thermoplastics are available in the market with a variety of properties suitable for different engineering applications, and few of those are available in a not yet polymerised form suitable for resin infusion. The proper selection of a new resin system among these thermoplastic polymers is a concern for manufactures in the current scenario and a special mathematical tool would be beneficial. In this paper, the authors introduce a new decision making tool for resin selection based on significant attributes. This article provides a broad overview of suitable thermoplastic material systems for vacuum infusion process available in today’s market. An illustrative example—resin selection for vacuum infused of a wind turbine blade—is shown to demonstrate the intricacies involved in the proposed methodology for resin selection.

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