A COMBINED TEM/FIM EXAMINATION OF FIELD EMISSION AS A FIM SPECIMEN PREPARATION TECHNIQUE

1986 ◽  
Vol 47 (C7) ◽  
pp. C7-459-C7-462 ◽  
Author(s):  
M. G. BURKE ◽  
D. D. SIELOFF ◽  
S. S. BRENNER
Author(s):  
M. Talianker ◽  
D.G. Brandon

A new specimen preparation technique for visualizing macromolecules by conventional transmission electron microscopy has been developed. In this technique the biopolymer-molecule is embedded in a thin monocrystalline gold foil. Such embedding can be performed in the following way: the biopolymer is deposited on an epitaxially-grown thin single-crystal gold film. The molecule is then occluded by further epitaxial growth. In such an epitaxial sandwich an occluded molecule is expected to behave as a crystal-lattice defect and give rise to contrast in the electron microscope.The resolution of the method should be limited only by the precision with which the epitaxially grown gold reflects the details of the molecular structure and, in favorable cases, can approach the lattice resolution limit.In order to estimate the strength of the contrast due to the void-effect arising from occlusion of the DNA-molecule in a gold crystal some calculations were performed.


Author(s):  
F. Thoma ◽  
TH. Koller

Under a variety of electron microscope specimen preparation techniques different forms of chromatin appearance can be distinguished: beads-on-a-string, a 100 Å nucleofilament, a 250 Å fiber and a compact 300 to 500 Å fiber.Using a standardized specimen preparation technique we wanted to find out whether there is any relation between these different forms of chromatin or not. We show that with increasing ionic strength a chromatin fiber consisting of a row of nucleo- somes progressively folds up into a solenoid-like structure with a diameter of about 300 Å.For the preparation of chromatin for electron microscopy the avoidance of stretching artifacts during adsorption to the carbon supports is of utmost importance. The samples are fixed with 0.1% glutaraldehyde at 4°C for at least 12 hrs. The material was usually examined between 24 and 48 hrs after the onset of fixation.


Author(s):  
Jayesh Bellare

Seeing is believing, but only after the sample preparation technique has received a systematic study and a full record is made of the treatment the sample gets.For microstructured liquids and suspensions, fast-freeze thermal fixation and cold-stage microscopy is perhaps the least artifact-laden technique. In the double-film specimen preparation technique, a layer of liquid sample is trapped between 100- and 400-mesh polymer (polyimide, PI) coated grids. Blotting against filter paper drains excess liquid and provides a thin specimen, which is fast-frozen by plunging into liquid nitrogen. This frozen sandwich (Fig. 1) is mounted in a cooling holder and viewed in TEM.Though extremely promising for visualization of liquid microstructures, this double-film technique suffers from a) ireproducibility and nonuniformity of sample thickness, b) low yield of imageable grid squares and c) nonuniform spatial distribution of particulates, which results in fewer being imaged.


Author(s):  
S.R. Glanvill

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.


Author(s):  
William P. Wergin ◽  
Eric F. Erbe ◽  
Terrence W. Reilly

Although the first commercial scanning electron microscope (SEM) was introduced in 1965, the limited resolution and the lack of preparation techniques initially confined biological observations to relatively low magnification images showing anatomical surface features of samples that withstood the artifacts associated with air drying. As the design of instrumentation improved and the techniques for specimen preparation developed, the SEM allowed biologists to gain additional insights not only on the external features of samples but on the internal structure of tissues as well. By 1985, the resolution of the conventional SEM had reached 3 - 5 nm; however most biological samples still required a conductive coating of 20 - 30 nm that prevented investigators from approaching the level of information that was available with various TEM techniques. Recently, a new SEM design combined a condenser-objective lens system with a field emission electron source.


Author(s):  
R.T. Blackham ◽  
J.J. Haugh ◽  
C.W. Hughes ◽  
M.G. Burke

Essential to the characterization of materials using analytical electron microscopy (AEM) techniques is the specimen itself. Without suitable samples, detailed microstructural analysis is not possible. Ultramicrotomy, or diamond knife sectioning, is a well-known mechanical specimen preparation technique which has been gaining attention in the materials science area. Malis and co-workers and Glanvill have demonstrated the usefulness and applicability of this technique to the study of a wide variety of materials including Al alloys, composites, and semiconductors. Ultramicrotomed specimens have uniform thickness with relatively large electron-transparent areas which are suitable for AEM anaysis.Interface Analysis in Type 316 Austenitic Stainless Steel: STEM-EDS microanalysis of grain boundaries in austenitic stainless steels provides important information concerning the development of Cr-depleted zones which accompany M23C6 precipitation, and documentation of radiation induced segregation (RIS). Conventional methods of TEM sample preparation are suitable for the evaluation of thermally induced segregation, but neutron irradiated samples present a variety of problems in both the preparation and in the AEM analysis, in addition to the handling hazard.


Author(s):  
K. Doong ◽  
J.-M. Fu ◽  
Y.-C. Huang

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.


2021 ◽  
pp. 175815592098715
Author(s):  
José Carrillo-Ortiz ◽  
Santi Guallar ◽  
Jessica Martínez-Vargas ◽  
Javier Quesada

The methods used to preserve bird skins in museums have a potentially crucial impact on the feasibility and use of these specimens as a source of biological knowledge, although this subject is rarely broached. Study skins of birds are usually prepared with folded wings and straight legs to facilitate storage in the collection; yet, this method can hamper the measurement and examination of certain important features such as wing-feather moult. To make consultation easier for ornithologists, alternative preparation methods such as the splitting of wings and tarsi from the rest of the animal have been proposed by curators. Our aim was to study whether or not preparing bird specimens with spread limbs makes consultation simpler. First, we used two different methods to prepare two specimens each of two common European passerine species: (1) ‘traditional’ (folded wings and straight tarsi) and (2) ‘spread’ (limbs spread on one side of the body). Then, we asked 22 experienced ornithologists to identify moult limits and take three biometric measurements (wing chord, length of the third primary feather and tarsus length) from all four specimens. Subsequently, we asked which preparation method they preferred for obtaining data. The ‘spread’ preparation was preferred for moult, third primary feather length and tarsus length, whilst the ‘traditional’ preparation was preferred for wing chord. Data obtained from the folded and spread preparations were very highly repeatable within each method but only moderately to highly repeatable between methods. One of the handicaps with the ‘spread’ preparation is the increase in storage space required, a factor that should be taken into account before it is employed. Nevertheless, this specimen preparation technique can greatly facilitate consultation and therefore improve the scientific value of ornithological collections.


1991 ◽  
Vol 254 ◽  
Author(s):  
Helen L. Humiston ◽  
Bryan M. Tracy ◽  
M. Lawrence ◽  
A. Dass

AbstractAn alternative VLSI TEM specimen preparation technique has been developed to produce 100μm diameter electron transparent thin area by using a conventional dimpler with a texmet padded ‘flatting tool’ for dimpling and a microcloth padded ‘flatting tool’ for polishing, followed by low angle ion milling. The advantages of this technique are a large sampling area and shorter milling times than conventional specimen preparation methods. In the following, we report the details of the modified dimpling technique. The improvements in available electron transparency, and a decrease in ion milling time are demonstrated with the preparation of planar and cross section VLSI device samples.


Author(s):  
Khalid Al-Shibli ◽  
Emir José Macari ◽  
Stein Sture

This study focuses on the use of digital image techniques to evaluate and develop quantitative measures of fabric for fine-grained granular materials to assess degrees of homogeneity and isotropy. The description of a procedure performed to prepare homogeneous cylindrical sand specimens is presented. Two techniques were performed to investigate the homogeneity. The specimens were preserved with an ultralow viscosity embedding epoxy resin, and they were allowed to cure prior to dissection for subsequent detailed analysis of the internal fabric. Digital imaging techniques were used to process and analyze various sections of the specimens. The analysis consisted of studying two specific fabric characteristics of the soil: particle orientation and local void ratio. Frequency distribution charts were plotted to assess the degrees of homogeneity and isotropy. Other invasive techniques were also used in some cases to assess the repeatability of the specimen preparation technique. Results indicate that the specimens were prepared with a high degree of homogeneity. Some degree of spatial variation was observed in the local void ratio evaluation.


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