• Applied Microscopy
• /
• v.44 no.4
• /
• pp.133-137
• /
• 2014

We suggest a facile transmission electron microscopy (TEM) specimen preparation method for the direct (polymer-free) transfer of layer-area graphene from Cu substrates to a TEM grid. The standard (polymer-based) method and direct transfer method were by TEM, high-resolution TEM, and energy dispersive X-ray spectroscopy (EDS). The folds and crystalline particles were formed in a graphene specimen by the standard method, while the graphene specimen by the direct method with a new etchant solution exhibited clean and full coverage of the graphene surface, which reduced several wet chemical steps and accompanying mechanical stresses and avoided formation of the oxide metal.

• Applied Microscopy
• /
• v.48 no.2
• /
• pp.49-53
• /
• 2018

A successful transmission electron microscope (TEM) analysis is closely related to the preparation of the TEM specimen and should be followed by the suitable TEM specimen preparation depending on the purpose of analysis and the subject materials. In the case of the Si-based anode material, lithium atoms of formed Li silicide were removed due to ion beam and electron beam during TEM specimen preparation and TEM observation. To overcome the problem, we proposed a new technique to make a TEM specimen without the ion beam damage. In this study, two types of test specimens from the Si-based anode material of Li-ion battery were prepared by respectively adopting the only focused ion beam (FIB) method and the new FIB-ultramicrotome method. TEM analyses of two samples were conducted to compare the Ga ion damage of the test specimen.

• Applied Microscopy
• /
• v.32 no.4
• /
• pp.311-317
• /
• 2002

There is great requirement on the TEM specimen preparation method with particle size selectivity as a prerequisite for the quantitative structure analysis on the materials such as gibbsite powder, which generally forms a large agglomerate and shows a variation of transition process depending on their sizes. In this experiment, we made an attempt to give a methodology for the TEM specimen preparation of powder with the size selectivity. After mixing 1 wt% gibbsite powder with ethanol solvent, gibbsite suspension was prepared by application of ball-milling and ultrasonification with addition of 0.25 vol% dispersion agent, Darvan C, which was diluted into distilled water by the ratio 1:19. Appling the static sedimentation method to gibbsite suspension after estimation of the sedimentation time by the measurement of accumulative concentration variation, we acquired TEM specimens with well-dispersed and size selected gibbsite particles in nm scale. Overall picture of each sample was taken by SEM and morphology of each dispersed particle was imaged by TEM. Raw and processed gibbsite powders were also examined by XRD to investigate whether they were suffered from phase change during the process or not.

• Applied Microscopy
• /
• v.46 no.2
• /
• pp.110-115
• /
• 2016

Transmission electron microscopy (TEM) is a powerful tool for analyzing a broad range of materials and provides localized information about the microstructure. However, the analysis results are strongly influenced by the quality of the thin foil specimen. Sample preparation for TEM analysis requires considerable skill, especially when the area of interest is small or the material of interest is difficult to thin because of its high hardness and its mechanical instability when thinned. This article selectively reviews recent advances in TEM sample preparation techniques using a tripod polisher. In particular, it introduces two typical types (fl at type and wedge type) of TEM sample preparation and the benefits and drawbacks of each method; finally, a method of making better samples for TEM analysis is suggested.

• Applied Microscopy
• /
• v.48 no.4
• /
• pp.122-125
• /
• 2018

The focused ion beam (FIB) method is widely used to prepare specimens for observation by transmission electron microscopy (TEM), which offers a wide variety of imaging and analytical techniques. TEM has played a significant role in material investigation. However, the FIB method induces amorphization due to bombardment with the high-energy gallium ($Ga^+$) ion beam. To solve this problem, electron beam induced deposition (EBID) is used to form a protective layer to prevent damage to the specimen surface. In this study, we introduce an optimized TEM specimen preparation procedure by comparing the EBID of carbon and tungsten as protective layers in FIB. The selection of appropriate EBID conditions for preparing specimens for TEM analysis is described in detail.

• Applied Microscopy
• /
• v.39 no.3
• /
• pp.277-281
• /
• 2009

Practical difficulties for preparing a good crosssectional specimen of GaN-based materials for transmission electron microscopy have arisen due to large difference of mechanical properties between hard ceramic substrate and soft GaN-layered materials. Uneven polishing, sudden cracking, delamination, and selective sputtering during the conventional wedge polishing technique are often encountered as experimental hindrances. The preparation technique based on Strecker's method can be applied to overcome these difficulties, which eventually leads to mechanically stable TEM samples independent of the mechanical properties of materials. The basic idea is to use hard ceramic dummy filler for embedding the sample of interest into the dummy frame. In this study, we applied this technique into preparing cross-sectional TEM specimen of the GaN-based materials with mechanical instability and demonstrated usefulness of this hard dummy filler method in which the possible modifications of the sample of interest during the preparation must be avoidable. In addition, practical precautions during the preparation were discussed.

• Applied Microscopy
• /
• v.45 no.4
• /
• pp.195-198
• /
• 2015

Gas-assisted etching (GAE) with focused ion beam (FIB) was applied to prepare plan-view specimens of Cu thin-layer on a silicon substrate for transmission electron microscopy (TEM). GAE using $XeF_2$ gas selectively etched the silicon substrate without volume loss of the Cu thin-layer. The plan-view specimen of the Cu thin film prepared by FIB milling with GAE was observed by scanning electron microscopy and $C_S$-corrected high-resolution TEM to estimate the size and microstructure of the TEM specimen. The GAE with FIB technique overcame various artifacts of conventional FIB milling technique such as bending, shrinking and non-uniform thickness of the TEM specimens. The Cu thin film was uniform in thickness and relatively larger in size despite of the thickness of <200 nm.

• Applied Microscopy
• /
• v.29 no.4
• /
• pp.493-498
• /
• 1999

With increasing demand for fast and reliable, yet economical data storage devices, the role of optical disk technology is becoming more important. In recent years, advanced laser technology combined with new materials has given the competitive edge over the traditional magnetic memory devices both in memory capacity and reliability of data retrieval. Continuing effort is being put into developing smaller and more complex structures for optical disks to increase their memory density. Characterization of such multilayered structure requires not only high spatial resolution for observation but also laborious specimen preparation. In this paper, the method of preparing optical disk specimens for TEM characterization is described in detail. The microstructural features in optical disks observed by TEM are also discussed.

• Applied Microscopy
• /
• v.29 no.1
• /
• pp.67-73
• /
• 1999

It is practically hard to prepare good TEM specimens from powders which are embedded in epoxy materials for ion milling, because the milling rate difference between powders and epoxy is quite large. In order to overcome this problem, we tried to find methods to increase the density of powders in the embedding epoxy without loosing the adhesive strength between them. Powder density was considerably increased by employing a centrifuge for embedding, compared to the result by a conventional vacuum embedding. In addition, mixing powders of different sizes after sieving also enhanced the final density by allowing smaller particles filling in the gaps of larger particles. Ion milling of powders embedded by these methods resulted in thin specimens good enough for normal TEM works. TEM specimens from spherical, platy and fibrous powders of submicron size were successfully prepared by this centrifuging method.

• Applied Microscopy
• /
• v.28 no.3
• /
• pp.315-328
• /
• 1998

The present study was carried out to investigate the effect of ultrasonic bath in tissue preparation for transmission electron microscopy. The method used standard reagents and media, and employed ultrasonic bath agitation to accelerate fluid exchange. The liver kidney, stomach and cardiac muscle tissues of male Sprague-Dawley rats were used for the experiment, and the experimental design was divided into 4 groups; The control group using rotators (Traditional method, 1,625 mins) and the three experimental groups using ultrasonic bath (UB) in the primary fixation through the infiltration processes (UB I; 62.5 mins, UB II; 125 mins, UB III; 250 mins). The results were as follows; 1. In the control group, tissues were easily sectioned, and showed well preserved intact membranes, and cell organelles such as mitochondria, lysosome, peroxisome, rough endoplasmic reticulum and smooth endoplasmic reticulum. 2. In the UB treated group I, tissues showed holes due to the inadequate removal of both water and fluids used in the dehydration process. Also the mitochondria of cell organelles, especially, showed swollen intracristal spaces and dense matrices due to poor fixation. 3. In the UB treated group II, tissues showed good preservation of cell organelles and specimen slice sections. Also, no holes were observed. 4. In the UB treated group III, tissues showed leaching of structural components in the cytoplasm, but no holes were observed. In conclusion, the ultrasonic bath procedure takes approximately 120 minutes from specimen fixation to resin infiltration and gives excellent results.