Preparation of cross-sectional samples for near-surface TEM studies

Author(s):  
R.C. Dickenson ◽  
K.R. Lawless

In thermal oxidation studies, the structure of the oxide-metal interface and the near-surface region is of great importance. A technique has been developed for constructing cross-sectional samples of oxidized aluminum alloys, which reveal these regions. The specimen preparation procedure is as follows: An ultra-sonic drill is used to cut a 3mm diameter disc from a 1.0mm thick sheet of the material. The disc is mounted on a brass block with low-melting wax, and a 1.0mm hole is drilled in the disc using a #60 drill bit. The drill is positioned so that the edge of the hole is tangent to the center of the disc (Fig. 1) . The disc is removed from the mount and cleaned with acetone to remove any traces of wax. To remove the cold-worked layer from the surface of the hole, the disc is placed in a standard sample holder for a Tenupol electropolisher so that the hole is in the center of the area to be polished.

Author(s):  
Ryan D. Evans

Transmission electron microscopy (TEM) was performed on cross-sectional samples from tapered roller bearing cone raceways. The bearings were tested in mineral oil with and without sulfur- and phosphorus-containing gear oil additives. Focused ion beam techniques were used for TEM specimen preparation. Imaging, electron diffraction, and x-ray energy dispersive spectroscopy revealed the structure and composition of near surface material (depth < 500 nm) and surface layers.


Author(s):  
А.И. Баранов ◽  
Д.А. Кудряшов ◽  
А.В. Уваров ◽  
И.А. Морозов ◽  
А.А. Максимова ◽  
...  

The possibility of using admittance spectroscopy to characterization the quality of ITO/MoOx/n-Si structures is shown. It has been demonstrated that magnetron sputtering of ITO layer at room temperature leads to radiation defects formation in the near-surface region of Si near the MoOx/Si interface with a depth of 0.13 and 0.26 eV below the conduction band with a capture cross-sectional area of (1–5)∙10^-19 and (5–10)∙10^-19 cm^-2, respectively. An increase in the deposition temperature of the ITO layer to 130 °C allows to reduce the concentration below the sensitivity leading to a significant improvement of solar cells characteristic.


Author(s):  
D. N. Braski ◽  
P. D. Goodell ◽  
J. V. Cathcart ◽  
R. H. Kane

It has been known for some time that the addition of small oxide particles to an 80 Ni—20 Cr alloy not only increases its elevated-temperature strength, but also markedly improves its resistance to oxidation. The mechanism by which the oxide dispersoid enhances the oxidation resistance is being studied collaboratively by ORNL and INCO Alloy Products Company.Initial experiments were performed using INCONEL alloy MA754, which is nominally: 78 Ni, 20 Cr, 0.05 C, 0.3 Al, 0.5 Ti, 1.0 Fe, and 0.6 Y2O3 (wt %).Small disks (3 mm diam × 0.38 mm thick) were cut from MA754 plate stock and prepared with two different surface conditions. The first was prepared by mechanically polishing one side of a disk through 0.5 μm diamond on a syntron polisher while the second used an additional sulfuric acid-methanol electropolishing treatment to remove the cold-worked surface layer. Disks having both surface treatments were oxidized in a radiantly heated furnace for 30 s at 1000°C. Three different environments were investigated: hydrogen with nominal dew points of 0°C, —25°C, and —55°C. The oxide particles and films were examined in TEM by using extraction replicas (carbon) and by backpolishing to the oxide/metal interface. The particles were analyzed by EDS and SAD.


Author(s):  
A. K. Rai ◽  
P. P. Pronko

Several techniques have been reported in the past to prepare cross(x)-sectional TEM specimen. These methods are applicable when the sample surface is uniform. Examples of samples having uniform surfaces are ion implanted samples, thin films deposited on substrates and epilayers grown on substrates. Once device structures are fabricated on the surfaces of appropriate materials these surfaces will no longer remain uniform. For samples with uniform surfaces it does not matter which part of the surface region remains in the thin sections of the x-sectional TEM specimen since it is similar everywhere. However, in order to study a specific region of a device employing x-sectional TEM, one has to make sure that the desired region is thinned. In the present work a simple way to obtain thin sections of desired device region is described.


Author(s):  
S. H. Chen

Sn has been used extensively as an n-type dopant in GaAs grown by molecular-beam epitaxy (MBE). The surface accumulation of Sn during the growth of Sn-doped GaAs has been observed by several investigators. It is still not clear whether the accumulation of Sn is a kinetically hindered process, as proposed first by Wood and Joyce, or surface segregation due to thermodynamic factors. The proposed donor-incorporation mechanisms were based on experimental results from such techniques as secondary ion mass spectrometry, Auger electron spectroscopy, and C-V measurements. In the present study, electron microscopy was used in combination with cross-section specimen preparation. The information on the morphology and microstructure of the surface accumulation can be obtained in a fine scale and may confirm several suggestions from indirect experimental evidence in the previous studies.


Author(s):  
K. F. Russell ◽  
L. L. Horton

Beams of heavy ions from particle accelerators are used to produce radiation damage in metal alloys. The damaged layer extends several microns below the surface of the specimen with the maximum damage and depth dependent upon the energy of the ions, type of ions, and target material. Using 4 MeV heavy ions from a Van de Graaff accelerator causes peak damage approximately 1 μm below the specimen surface. To study this area, it is necessary to remove a thickness of approximately 1 μm of damaged metal from the surface (referred to as “sectioning“) and to electropolish this region to electron transparency from the unirradiated surface (referred to as “backthinning“). We have developed electropolishing techniques to obtain electron transparent regions at any depth below the surface of a standard TEM disk. These techniques may be applied wherever TEM information is needed at a specific subsurface position.


Author(s):  
Julia T. Luck ◽  
C. W. Boggs ◽  
S. J. Pennycook

The use of cross-sectional Transmission Electron Microscopy (TEM) has become invaluable for the characterization of the near-surface regions of semiconductors following ion-implantation and/or transient thermal processing. A fast and reliable technique is required which produces a large thin region while preserving the original sample surface. New analytical techniques, particularly the direct imaging of dopant distributions, also require good thickness uniformity. Two methods of ion milling are commonly used, and are compared below. The older method involves milling with a single gun from each side in turn, whereas a newer method uses two guns to mill from both sides simultaneously.


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):  
H.-J. Ou ◽  
J. M. Cowley ◽  
A. A. Higgs

A scanning ion gun system has been installed on the specimen preparation chamber (pressure ∼5xl0-8 torr) of the VG-HB5 STEM microscope. By using the specimen current imaging technique, it is possible to use an ion beam to sputter-clean the preferred surface region on a bulk sample. As shown in figure 1, the X-Y raster-gate control of the scanning unit for the Krato Mini-Beam I is used to minimize the beam raster area down to a 800μm x800μm square region. With beam energy of 2.5KeV, the MgO cleavage surface has been ion sputter-cleaned for less than 1 minute. The carbon film or other contaminant, introduced during the cleavage process in air, is mostly removed from the MgO crystal surfaces.The immediate SREM inspection of this as-cleaned MgO surface, within the adjacent STEM microscope, has revealed the detailed surface structures of atomic steps, which were difficult to observe on the as-cleaved MgO surfaces in the previous studies.


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