An Aldehyde/Hydrazide Polymerization Technique for Biological SEM Specimen Preparation

1981 ◽  
Vol 39 ◽  
pp. 644-645
Author(s):  
W. T. Gunning ◽  
R. E. Crang
Keyword(s):  
Electron Microscopy ◽  
Freeze Drying ◽  
Water Soluble ◽  
Specimen Preparation ◽  
Crystal Formation ◽  
Ice Crystal ◽  
Polymer Medium ◽  
Low Contrast ◽  
Transmission Electron ◽  
Limited Application

Two water-soluble embedding techniques for transmission electron microscopy (TEM) utilizing the polymerization of glutaraldehyde were proposed in the early 1970's. Pease and Peterson introduced a glutaraldehyde-urea polymer medium and Heckman and Barrnett proposed a glutaraldehyde-carbohydrazide (GACH) medium. Both permitted the retention of lipids in tissues without the harsh extraction of cellular constituents by fixatives, organic dehydrators and embedding agents. These techniques were of limited application and yielded low contrast or negative-stained images in the TEM. This technique has not been previously considered as potentially useful for scanning electron microscopy (SEM) due to the covering and obliterating of surface morphology. Virtually all SEM techniques for biological and specimen preparation, aside from freeze-drying, replace or extract most of the native elemental compositions of cells and tissues. Freezing and freeze-drying techniques are cumbersome, time-consuming, may require elaborate equipment and can induce artifacts due to ice crystal formation. We propose a new approach of SEM sample preparation using modifications of the GACH technique employed in TEM.

The Critical Point Drying Method Applied to Scanning Electron Microscopy of L-929 Cells

1970 ◽  
Vol 28 ◽  
pp. 278-279
Author(s):  
Charles TurnbiLL ◽  
Delbert E. Philpott
Keyword(s):  
Electron Microscopy ◽  
Carbon Dioxide ◽  
Surface Tension ◽  
Critical Point ◽  
Freeze Drying ◽  
Attractive Alternative ◽  
Crystal Formation ◽  
Critical Point Drying ◽  
Time Required ◽  
Scanning Electron

The advent of the scanning electron microscope (SCEM) has renewed interest in preparing specimens by avoiding the forces of surface tension. The present method of freeze drying by Boyde and Barger (1969) and Small and Marszalek (1969) does prevent surface tension but ice crystal formation and time required for pumping out the specimen to dryness has discouraged us. We believe an attractive alternative to freeze drying is the critical point method originated by Anderson (1951; for electron microscopy. He avoided surface tension effects during drying by first exchanging the specimen water with alcohol, amy L acetate and then with carbon dioxide. He then selected a specific temperature (36.5°C) and pressure (72 Atm.) at which carbon dioxide would pass from the liquid to the gaseous phase without the effect of surface tension This combination of temperature and, pressure is known as the "critical point" of the Liquid.

Direct Observation of Heat Exchanger Deposits by Cross Sectioning

1967 ◽  
Vol 25 ◽  
pp. 364-365
Author(s):  
R. W. Anderson ◽  
D. L. Senecal
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Heat Exchanger ◽  
Direct Observation ◽  
Cross Sections ◽  
Preparation Method ◽  
Specimen Preparation ◽  
Flowing Water ◽  
Transmission Electron ◽  
Deposit Layer

A problem was presented to observe the packing densities of deposits of sub-micron corrosion product particles. The deposits were 5-100 mils thick and had formed on the inside surfaces of 3/8 inch diameter Zircaloy-2 heat exchanger tubes. The particles were iron oxides deposited from flowing water and consequently were only weakly bonded. Particular care was required during handling to preserve the original formations of the deposits. The specimen preparation method described below allowed direct observation of cross sections of the deposit layers by transmission electron microscopy.The specimens were short sections of the tubes (about 3 inches long) that were carefully cut from the systems. The insides of the tube sections were first coated with a thin layer of a fluid epoxy resin by dipping. This coating served to impregnate the deposit layer as well as to protect the layer if subsequent handling were required.

Transmission Electron Microscopy of an Aluminum-Silver-Stainless Steel Solid State Bond

1985 ◽  
Vol 43 ◽  
pp. 172-173
Author(s):  
M. J. Carr ◽  
J. F. Shewbridge ◽  
T. O. Wilford
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Solid State ◽  
Specimen Preparation ◽  
Dimensional Control ◽  
Tem Analysis ◽  
Metal Parts ◽  
Dissimilar Metal ◽  
Transmission Electron ◽  
Short Time

Strong solid state bonds are routinely produced between physical vapor deposited (PVD) silver coatings deposited on sputter cleaned surfaces of two dissimilar metal parts. The low temperature (200°C) and short time (10 min) used in the bonding cycle are advantageous from the standpoint of productivity and dimensional control. These conditions unfortunately produce no microstructural changes at or near the interface that are detectable by optical, SEM, or microprobe examination. Microstructural problems arising at these interfaces could therefore easily go undetected by these techniques. TEM analysis has not been previously applied to this problem because of the difficulty in specimen preparation. The purpose of this paper is to describe our technique for preparing specimens from solid state bonds and to present our initial observations of the microstructural details of such bonds.

Transmission Electron Microscopy (TEM) Specimen Preparation Technique using Focused Ion Beam (FIB): Application to Material Characterization of Chemical Vapor Deposition of Tungsten (W) and Tungsten Silicides (WSix)

1997 ◽  
Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Chemical Vapor Deposition ◽  
Vapor Deposition ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Chemical Vapor ◽  
Specimen Preparation ◽  
Preparation Technique ◽  
Transmission Electron

Abstract The specimen preparation technique using focused ion beam (FIB) to generate cross-sectional transmission electron microscopy (XTEM) samples of chemical vapor deposition (CVD) of Tungsten-plug (W-plug) and Tungsten Silicides (WSix) was studied. Using the combination method including two axes tilting[l], gas enhanced focused ion beam milling[2] and sacrificial metal coating on both sides of electron transmission membrane[3], it was possible to prepare a sample with minimal thickness (less than 1000 A) to get high spatial resolution in TEM observation. Based on this novel thinning technique, some applications such as XTEM observation of W-plug with different aspect ratio (I - 6), and the grain structure of CVD W-plug and CVD WSix were done. Also the problems and artifacts of XTEM sample preparation of high Z-factor material such as CVD W-plug and CVD WSix were given and the ways to avoid or minimize them were suggested.

A Methodology to Reduce Ion Beam Induced Damage in TEM Specimens Prepared by FIB

2002 ◽  
Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Sensitive Issue ◽  
Transmission Electron

Abstract Focused ion beam (FIB) has become a useful tool in the Integrated Circuit (IC) industry, It is playing an important role in Failure Analysis (FA), circuit repair and Transmission Electron Microscopy (TEM) specimen preparation. In particular, preparation of TEM samples using FIB has become popular within the last ten years [1]; the progress in this field is well documented. Given the usefulness of FIB, “Artifact” however is a very sensitive issue in TEM inspections. The ability to identify those artifacts in TEM analysis is an important as to understanding the significance of pictures In this paper, we will describe how to measure the damages introduced by FIB sample preparation and introduce a better way to prevent such kind of artifacts.

Synthesis and Characterization of Water-Soluble Monolayer-Protected Gold Nanoparticles

2011 ◽  
Vol 415-417 ◽  
pp. 617-620 ◽  
Author(s):  
Yan Su ◽  
Ying Yun Lin ◽  
Yu Li Fu ◽  
Fan Qian ◽  
Xiu Pei Yang ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Particle Size ◽  
Gold Nanoparticles ◽  
Average Particle Size ◽  
Water Soluble ◽  
Synthesis And Characterization ◽  
Average Particle ◽  
Transmission Electron

Water-soluble gold nanoparticles (AuNPs) were prepared using 2-mercapto-4-methyl-5- thiazoleacetic acid (MMTA) as a stabilizing agent and sodium borohydride (NaBH4) as a reducing agent. The AuNPs product was analyzed by transmission electron microscopy (TEM), UV-vis absorption spectroscopy and Fourier transform infrared spectroscopy (FTIR). The TEM image shows that the particles were well-dispersed and their average particle size is about 5 nm. The UV-vis absorption and FTIR spectra confirm that the MMTA-AuNPs was stabilized by the carboxylate ions present on the surface of the AuNPs.

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.

Recent Developments in Mechanical Specimen Preparation for Tem and Sem Applications

1999 ◽  
Vol 5 (S2) ◽  
pp. 932-933
Author(s):  
W. Li ◽  
S. Q. Wang ◽  
R. Trussell ◽  
M. Xu ◽  
R.D. Venables ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Integrated Circuits ◽  
Sample Preparation ◽  
Ion Beam ◽  
Wedge Angle ◽  
Specimen Preparation ◽  
Precise Control ◽  
Transmission Electron ◽  
Recent Developments ◽  
Polishing Tool

The continued reduction in the size of critical features in integrated circuits has resulted in the need to develop rapid, site-specific, sectioning techniques to enable efficient physical characterization of the structures of interest. We have implemented a mechanical polishing approach to achieve this objective with the additional goals of maximizing the number of targeted sites in a sample that can be analyzed, and minimizing physically destructive procedures, such as ion beam exposure. Precision sample preparation approaches have been under investigation for both transmission electron microscopy and scanning electron microscopy.The mechanical specimen preparation approach used in this work is a variant of the well-known wedge polishing technique. Here we use a polishing tool that does not contact the grinding surface, thus allowing precise control of the wedge angle. Prior to sample preparation, the polishing tool head was precision aligned parallel to the platen.

Facile synthesis of water-soluble graphene-based composite: Non-covalently functionalized with chitosan-ionic liquid conjugation

2016 ◽  
Vol 09 (03) ◽  
pp. 1650045 ◽  
Author(s):  
Pei-Ying Li ◽  
Kai-Yu Cheng ◽  
Xiu-Cheng Zheng ◽  
Pu Liu ◽  
Xiu-Juan Xu
Keyword(s):  
Electron Microscopy ◽  
Ionic Liquid ◽  
Chemical Reduction ◽  
Water Soluble ◽  
X Ray Diffraction ◽  
Facile Synthesis ◽  
X Ray ◽  
Transmission Electron ◽  
Vis Spectroscopy ◽  
Text Interaction

Chitosan-ionic liquid conjugation (CILC), which was prepared through the reaction of 1-(4-bromobutyl)-3-methylimidazolium bromide (BBMIB) with chitosan, was firstly used to prepare functionalized graphene composite via the chemical reduction of graphene oxide (GO). The obtained water soluble graphene-based composite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), ultraviolet-visible (UV–Vis) spectroscopy and so on. CILC-RGO showed excellent dispersion stability in water at the concentration of 2.0 mg/mL, which was stable for several months without any precipitate. This may be ascribed to the electrostatic attraction and [Formula: see text]–[Formula: see text] interaction between CILC and graphene.

A model for the composite nanostructure of bone suggested by high-resolution transmission electron microscopy

2003 ◽  
Vol 67 (6) ◽  
pp. 1171-1182 ◽  
Author(s):  
B. A. Cressey ◽  
G. Cressey
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
High Resolution ◽  
Preparation Method ◽  
Ion Beam ◽  
Human Bone ◽  
Specimen Preparation ◽  
Transmission Electron ◽  
Ancient Bone ◽  
Close Analogue

AbstractWe have imaged the spatially-preserved microtexture of biogenic apatite, retained together with its collagen template, in non-demineralized human bone using high-resolution transmission electron microscopy. Using ion-beam thinning, a specimen preparation method generally employed for inorganic minerals rather than for biological materials, we have imaged a composite nanostructure of bone not previously reported, and we propose a model for this nano-architecture that involves a boxconstruction of apatite plates and apatite sheets. This observation provides a new understanding of bone strength at the nanometre scale and suggests how post mortem enhancement of this texture by recrystallization probably accounts for the durability of ancient bone. Modern sheep bone (a close analogue for recently dead human bone) imaged in the same way also shows evidence of this composite architecture.

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