A modified specimen holder for cone calorimeter testing of composite materials to reduce influence from specimen edges

2021 ◽  
Author(s):  
Anna Sandinge ◽  
Per Blomqvist ◽  
Michael Rahm
Author(s):  
Russell L. Steere ◽  
Michael Moseley

A redesigned specimen holder and cap have made possible the freeze-etching of both fracture surfaces of a frozen fractured specimen. In principal, the procedure involves freezing a specimen between two specimen holders (as shown in A, Fig. 1, and the left side of Fig. 2). The aluminum specimen holders and brass cap are constructed so that the upper specimen holder can be forced loose, turned over, and pressed down firmly against the specimen stage to a position represented by B, Fig. 1, and the right side of Fig. 2.


Author(s):  
R.R. Russell

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.


Author(s):  
Louis T. Germinario

A liquid nitrogen stage has been developed for the JEOL JEM-100B electron microscope equipped with a scanning attachment. The design is a modification of the standard JEM-100B SEM specimen holder with specimen cooling to any temperatures In the range ~ 55°K to room temperature. Since the specimen plane is maintained at the ‘high resolution’ focal position of the objective lens and ‘bumping’ and thermal drift la minimized by supercooling the liquid nitrogen, the high resolution capability of the microscope is maintained (Fig.4).


Author(s):  
K.P.D. Lagerlof

Although most materials contain more than one phase, and thus are multiphase materials, the definition of composite materials is commonly used to describe those materials containing more than one phase deliberately added to obtain certain desired physical properties. Composite materials are often classified according to their application, i.e. structural composites and electronic composites, but may also be classified according to the type of compounds making up the composite, i.e. metal/ceramic, ceramic/ceramie and metal/semiconductor composites. For structural composites it is also common to refer to the type of structural reinforcement; whisker-reinforced, fiber-reinforced, or particulate reinforced composites [1-4].For all types of composite materials, it is of fundamental importance to understand the relationship between the microstructure and the observed physical properties, and it is therefore vital to properly characterize the microstructure. The interfaces separating the different phases comprising the composite are of particular interest to understand. In structural composites the interface is often the weakest part, where fracture will nucleate, and in electronic composites structural defects at or near the interface will affect the critical electronic properties.


Author(s):  
David C. Joy ◽  
Dennis M. Maher

High-resolution images of the surface topography of solid specimens can be obtained using the low-loss technique of Wells. If the specimen is placed inside a lens of the condenser/objective type, then it has been shown that the lens itself can be used to collect and filter the low-loss electrons. Since the probeforming lenses in TEM instruments fitted with scanning attachments are of this type, low-loss imaging should be possible.High-resolution, low-loss images have been obtained in a JEOL JEM 100B fitted with a scanning attachment and a thermal, fieldemission gun. No modifications were made to the instrument, but a wedge-shaped, specimen holder was made to fit the side-entry, goniometer stage. Thus the specimen is oriented initially at a glancing angle of about 30° to the beam direction. The instrument is set up in the conventional manner for STEM operation with all the lenses, including the projector, excited.


Author(s):  
Tokio Nei ◽  
Haruo Yotsumoto ◽  
Yoichi Hasegawa ◽  
Yuji Nagasawa

In order to observe biological specimens in their native state, that is, still containing their water content, various methods of specimen preparation have been used, the principal two of which are the chamber method and the freeze method.Using its recently developed cold stage for installation in the pre-evacuation chamber of a scanning electron microscope, we have succeeded in directly observing a biological specimen in its frozen state without the need for such conventional specimen preparation techniques as drying and metallic vacuum evaporation. (Echlin, too, has reported on the observation of surface structures using the same freeze method.)In the experiment referred to herein, a small sliced specimen was place in the specimen holder. After it was rapidly frozen by freon cooled with liquid nitrogen, it was inserted into the cold stage of the specimen chamber.


Author(s):  
William P. Wergin ◽  
Eric F. Erbe ◽  
Eugene L. Vigil

Investigators have long realized the potential advantages of using a low temperature (LT) stage to examine fresh, frozen specimens in a scanning electron microscope (SEM). However, long working distances (W.D.), thick sputter coatings and surface contamination have prevented LTSEM from achieving results comparable to those from TEM freeze etch. To improve results, we recently modified techniques that involve a Hitachi S570 SEM, an Emscope SP2000 Sputter Cryo System and a Denton freeze etch unit. Because investigators have frequently utilized the fractured E face of the plasmalemma of yeast, this tissue was selected as a standard for comparison in the present study.In place of a standard specimen holder, a modified rivet was used to achieve a shorter W.D. (1 to -2 mm) and to gain access to the upper detector. However, the additional height afforded by the rivet, precluded use of the standard shroud on the Emscope specimen transfer device. Consequently, the sample became heavily contaminated (Fig. 1). A removable shroud was devised and used to reduce contamination (Fig. 2), but the specimen lacked clean fractured edges. This result suggested that low vacuum sputter coating was also limiting resolution.


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