Preparation of Ceramic Particulates for Transmission Electron Microscopy

1980 ◽  
Vol 38 ◽  
pp. 196-197
Author(s):  
R. J. Lauf ◽  
H. Keating
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ceramic Materials ◽  
Ion Milling ◽  
Plastic Films ◽  
Transmission Electron ◽  
Specimen Orientation ◽  
Selection Of

The preparation of fragmented or particulate ceramic materials for transmission electron microscopy (TEM) examination has traditionally been difficult, particularly if a durable, permanent specimen is desired. Furthermore, most established methods for dealing with micron- and submicron-sized samples (e.g., dispersion in plastic films) do not permit selection of orientations or ion thinning. A technique has been developed that is useful for a variety of materials, permits the selection of specimen orientation, is compatible with ion milling requirements, and produces a durable specimen that can be reexamined later if necessary.

Preparation of Particulates for Transmission Electron Microscopy: An Update

1981 ◽  
Vol 39 ◽  
pp. 132-133
Author(s):  
R. J. Lauf ◽  
S. S. Rawlston
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Hot Pressing ◽  
Coal Fly Ash ◽  
Ceramic Materials ◽  
Dental Amalgam ◽  
Ion Milling ◽  
Vacuum Hot Pressing ◽  
Transmission Electron ◽  
Cylindrical Mold

A method for preparing fragmented or particulate ceramic materials for transmission electron microscopy (TEM) by embedding in a solid metal matrix such as aluminum, using vacuum hot-pressing at about 550°C, followed by mechanical thinning and ion milling, has been published. This technique is useful for most high-melting ceramic materials but may introduce thermal damage to low-melting materials or to hydrated minerals. We describe here two relatively simple techniques that can be carried out at room temperature and that do not require vacuum hot-pressing equipment.The first technique disperses the sample in a dental amalgam. Premeasured capsules contain the silver alloy powder and mercury in separate compartments. The capsule is opened and a small amount of sample is added. The capsule is then closed and compressed to release the mercury and agitated for 1 to 2 min. The material is removed from the capsule and tightly packed into a 3-mm-diam cylindrical mold for hardening overnight. The resulting pellet is then sliced and thinned as in the earlier method. Figure 1 shows a coal fly ash particle prepared by this technique.

Techniques for Transmission Electron Microscopy of Fiber-Matrix Interfaces in Aluminum Alloy-Boron Composites by Ion Erosio

1971 ◽  
Vol 29 ◽  
pp. 204-205
Author(s):  
G. G. Shaw
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Aluminum Alloy ◽  
Electron Beam ◽  
Pure Aluminum ◽  
Ion Milling ◽  
Transmission Electron ◽  
Fiber Matrix ◽  
Ion Erosion ◽  
Row Of Fibers

The morphology and composition of the fiber-matrix interface can best be studied by transmission electron microscopy and electron diffraction. For some composites satisfactory samples can be prepared by electropolishing. For others such as aluminum alloy-boron composites ion erosion is necessary.When one wishes to examine a specimen with the electron beam perpendicular to the fiber, preparation is as follows: A 1/8 in. disk is cut from the sample with a cylindrical tool by spark machining. Thin slices, 5 mils thick, containing one row of fibers, are then, spark-machined from the disk. After spark machining, the slice is carefully polished with diamond paste until the row of fibers is exposed on each side, as shown in Figure 1.In the case where examination is desired with the electron beam parallel to the fiber, preparation is as follows: Experimental composites are usually 50 mils or less in thickness so an auxiliary holder is necessary during ion milling and for easy transfer to the electron microscope. This holder is pure aluminum sheet, 3 mils thick.

Comparative Microstructures of Ion Milled and Electrochemically Thinned Composite Materials

1974 ◽  
Vol 32 ◽  
pp. 546-547
Author(s):  
R.R. Russell
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Composite Materials ◽  
Great Difficulty ◽  
Ion Milling ◽  
Transmission Electron ◽  
Ion Damage ◽  
Intermetallic Composite

Transmission electron microscopy of metallic/intermetallic composite materials is most challenging since the microscopist typically has great difficulty preparing specimens with uniform electron thin areas in adjacent phases. The application of ion milling for thinning foils from such materials has been quite effective. Although composite specimens prepared by ion milling have yielded much microstructural information, this technique has some inherent drawbacks such as the possible generation of ion damage near sample surfaces.

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.

Transmission Electron Microscopy of Semiconductor Based Products

1998 ◽  
Vol 523 ◽  
Author(s):  
John Mardinly ◽  
David W. Susnitzky
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Size Reduction ◽  
Specimen Preparation ◽  
Specimen Thickness ◽  
Ion Milling ◽  
Feature Size ◽  
Transmission Electron

AbstractThe demand for increasingly higher performance semiconductor products has stimulated the semiconductor industry to respond by producing devices with increasingly complex circuitry, more transistors in less space, more layers of metal, dielectric and interconnects, more interfaces, and a manufacturing process with nearly 1,000 steps. As all device features are shrunk in the quest for higher performance, the role of Transmission Electron Microscopy as a characterization tool takes on a continually increasing importance over older, lower-resolution characterization tools, such as SEM. The Ångstrom scale imaging resolution and nanometer scale chemical analysis and diffraction resolution provided by modem TEM's are particularly well suited for solving materials problems encountered during research, development, production engineering, reliability testing, and failure analysis. A critical enabling technology for the application of TEM to semiconductor based products as the feature size shrinks below a quarter micron is advances in specimen preparation. The traditional 1,000Å thick specimen will be unsatisfactory in a growing number of applications. It can be shown using a simple geometrical model, that the thickness of TEM specimens must shrink as the square root of the feature size reduction. Moreover, the center-targeting of these specimens must improve so that the centertargeting error shrinks linearly with the feature size reduction. To meet these challenges, control of the specimen preparation process will require a new generation of polishing and ion milling tools that make use of high resolution imaging to control the ion milling process. In addition, as the TEM specimen thickness shrinks, the thickness of surface amorphization produced must also be reduced. Gallium focused ion beam systems can produce hundreds of Ångstroms of amorphised surface silicon, an amount which can consume an entire thin specimen. This limitation to FIB milling requires a method of removal of amorphised material that leaves no artifact in the remaining material.

Microstructure of LaB6-base thick film resistors

1992 ◽  
Vol 7 (8) ◽  
pp. 2225-2229 ◽  
Author(s):  
Z.G. Li ◽  
P.F. Carcia ◽  
P.C. Donohue
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Thick Film ◽  
Surface Area ◽  
Ion Milling ◽  
Cross Sectional ◽  
Electrically Conductive ◽  
Transmission Electron ◽  
High Temperature Processing ◽  
Thin Wedge

The microstructure of LaB6-base thick film resistors was investigated by cross-sectional transmission electron microscopy. The specimens were prepared by a technique that polished them to a thin wedge, thus avoiding ion-milling and permitting imaging over a distance of tens of microns. The resistor microstructure contained a finely divided electrically conductive phase of TaB2 and nonconducting crystals of CaTa4O11, formed during high temperature processing of glass and LaB6 ingredients of the thick film ink. Using higher surface area ingredients virtually suppressed the formation of CaTa4O11 crystals, and the microstructure became more uniform. Resistors made with higher surface area intermediates also had better voltage withstanding properties.

scholarly journals TEM sample preparation for Li-ion secondary battery using ion slicer

2021 ◽  
Author(s):  
JungSik Park ◽  
Yoon-Jung Kang ◽  
SunEui Choi ◽  
YongNam Jo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Spherical Aberration ◽  
Lithium Ion ◽  
Ion Milling ◽  
Intrinsic Structure ◽  
Tem Analysis ◽  
Secondary Battery ◽  
Transmission Electron

Abstract The main purpose in this paper is a sample preparation of transmission electron microscopy (TEM) for the lithium-ion secondary battery in the form of micro-sized powders. To avoid artefacts of the TEM sample preparation, the use of ion slicer milling for thinning and maintaining the intrinsic structure is described. Argon-ion milling techniques have been widely examined to make the optimized specimen, which makes TEM analysis more reliable. In the past few years, the correction of spherical aberration (Cs) in scanning transmission electron microscopy (STEM) has been developing rapidly, that results in the direct observation with the atomic level resolution not only for the high acceleration voltage but also its deaccelerated voltage as well. Especially, low-kV application has been markedly increased that needs the sufficient-transparent specimen without the structural distortion during the process of the sample preparation. In this study, the sample preparation for the high-resolution STEM observation has been greatly accomplished and investigations of its crystal integrity are carried out by Cs-corrected STEM.

scholarly journals Interpretational challenges related to studies of chalk particle surfaces in scanning and transmission electron microscopy

2018 ◽  
Vol 66 ◽  
pp. 151-165
Author(s):  
Morten Leth Hjuler ◽  
Vidar Folke Hansen ◽  
Ida Lykke Fabricius
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Electron Beam ◽  
Carbon Film ◽  
Burial Depth ◽  
High Electron ◽  
Ion Milling ◽  
Transmission Electron ◽  
Thin Carbon ◽  
Acceleration Voltage

Scanning and transmission electron microscopy (SEM and TEM) are capable of characterising the morphology and structure of sub-micron size substances attached to chalk particle surfaces. Some characteristics, however, may originate from sample preparation or reflect interaction between sample and the electron beam. Misinterpretation of surface features may lead to wrong conclusions regarding grain surface properties and cementation level and thus to erroneous characterisation of hydrocarbon reservoirs with respect to e.g. wettability, mechanical strength and maximum burial depth. In SEM, conductive coatings may mask surface details or generate artificial ornamentations, and carbon adhesive discs may cause the chalk surface to be covered with a thin carbon film. Electron beam acceleration voltage controls the degree of detail revealed by the electron beam, but in SEM a high electron beam acceleration voltage may provoke bending or curling of ultrathin particles. Recent organic filaments may be confused with clay flakes, and authigenic non-carbonate minerals may have formed in the pore fluid and settled during fluid removal. In TEM, the high acceleration voltage may cause beam damage to calcite and transform the outermost atomic layers into Ca oxide. Thin graphite membranes observed by TEM may be contamination from the carbon film supporting the sample, and overlapping chalk particles in samples formed by drying of a suspension may give the impression of being cemented together. In TEM residual adhesive from the ion-milling process can be confused with cementation features.

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