Studies of the scanning ion beam sputter-cleaned MgO crystal surface by scanning reflection electron microscopy

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.

1999 ◽  
Vol 5 (S2) ◽  
pp. 516-517
Author(s):  
Lucille A. Giannuzzi

The focused ion beam (FIB) instrument has been developed and exploited by the microelectronics arena for specimen preparation for both scanning and transmission electron microscopy (TEM). The inception [1] and subsequent development [2] of the FIB TEM lift-out (LO) technique has enabled electron transparent membranes of generally uniform thickness to be produced for TEM analysis. The primary advantage of the FIB technique is that site specific cross sections (or plan view sections [3]) may be fabricated quickly and reproducibly. The FIB LO technique has been used extensively in our laboratory for a wide range of materials [4] and biological applications [5] which are summarized in figure 1.The FIB LO method consists of milling a series of trenches around an area of interest. Then the bulk sample is tilted up to ∼60 degrees to allow the beam to impinge on the lower portion of the specimen surface so that cuts can be made along the bottom edge and the lower 2/3 of the distance up one side of the specimen.


Author(s):  
G. G. Hembree ◽  
M. A. Otooni ◽  
J. M. Cowley

The formation of oxide structures on single crystal films of metals has been investigated using the REMEDIE system (for Reflection Electron Microscopy and Electron Diffraction at Intermediate Energies) (1). Using this instrument scanning images can be obtained with a 5 to 15keV incident electron beam by collecting either secondary or diffracted electrons from the crystal surface (2). It is particularly suited to studies of the present sort where the surface reactions are strongly related to surface morphology and crystal defects and the growth of reaction products is inhomogeneous and not adequately described in terms of a single parameter. Observation of the samples has also been made by reflection electron diffraction, reflection electron microscopy and replication techniques in a JEM-100B electron microscope.A thin single crystal film of copper, epitaxially grown on NaCl of (100) orientation, was repositioned on a large copper single crystal of (111) orientation.


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):  
L. Wan ◽  
R. F. Egerton

INTRODUCTION Recently, a new compound carbon nitride (CNx) has captured the attention of materials scientists, resulting from the prediction of a metastable crystal structure β-C3N4. Calculations showed that the mechanical properties of β-C3N4 are close to those of diamond. Various methods, including high pressure synthesis, ion beam deposition, chemical vapor deposition, plasma enhanced evaporation, and reactive sputtering, have been used in an attempt to make this compound. In this paper, we present the results of electron energy loss spectroscopy (EELS) analysis of composition and bonding structure of CNX films deposited by two different methods.SPECIMEN PREPARATION Specimens were prepared by arc-discharge evaporation and reactive sputtering. The apparatus for evaporation is similar to the traditional setup of vacuum arc-discharge evaporation, but working in a 0.05 torr ambient of nitrogen or ammonia. A bias was applied between the carbon source and the substrate in order to generate more ions and electrons and change their energy. During deposition, this bias causes a secondary discharge between the source and the substrate.


Author(s):  
H. Banzhof ◽  
I. Daberkow

A Philips EM 420 electron microscope equipped with a field emission gun and an external STEM unit was used to compare images of single crystal surfaces taken by conventional reflection electron microscopy (REM) and scanning reflection electron microscopy (SREM). In addition an angle-resolving detector system developed by Daberkow and Herrmann was used to record SREM images with the detector shape adjusted to different details of the convergent beam reflection high energy electron diffraction (CBRHEED) pattern.Platinum single crystal spheres with smooth facets, prepared by melting a thin Pt wire in an oxyhydrogen flame, served as objects. Fig. 1 gives a conventional REM image of a (111)Pt single crystal surface, while Fig. 2 shows a SREM record of the same area. Both images were taken with the (555) reflection near the azimuth. A comparison shows that the contrast effects of atomic steps are similar for both techniques, although the depth of focus of the SREM image is reduced as a result of the large illuminating aperture. But differences are observed at the lengthened images of small depressions and protrusions formed by atomic steps, which give a symmetrical contrast profile in the REM image, while an asymmetric black-white contrast is observed in the SREM micrograph. Furthermore the irregular structures which may be seen in the middle of Fig. 2 are not visible in the REM image, although it was taken after the SREM record.


1991 ◽  
Vol 223 ◽  
Author(s):  
Qin Fuguang ◽  
Yao Zhenyu ◽  
Ren Zhizhang ◽  
S.-T. Lee ◽  
I. Bello ◽  
...  

ABSTRACTDirect ion beam deposition of carbon films on silicon in the ion energy range of 15–500eV and temperature range of 25–800°C has been studied using mass selected C+ ions under ultrahigh vacuum. The films were characterized with X-ray photoelectron spectroscopy, Raman spectroscopy, and transmission electron microscopy and diffraction analysis. Films deposited at room temperature consist mainly of amorphous carbon. Deposition at a higher temperature, or post-implantation annealing leads to formation of microcrystalline graphite. A deposition temperature above 800°C favors the formation of microcrystalline graphite with a preferred orientation in the (0001) direction. No evidence of diamond formation was observed in these films.


2003 ◽  
Vol 762 ◽  
Author(s):  
Z.B. Zhou ◽  
G.M. Hadi ◽  
R.Q. Cui ◽  
Z.M. Ding ◽  
G. Li

AbstractBased on a small set of selected publications on the using of nanocrystalline silicon films (nc-Si) for solar cell from 1997 to 2001, this paper reviews the application of nc-Si films as intrinsic layers in p-i-n solar cells. The new structure of nc-Si films deposited at high chamber pressure and high hydrogen dilution have characters of nanocrystalline grains with dimension about several tens of nanometer embedded in matrix of amorphous tissue and a high volume fraction of crystallinity (60~80%). The new nc-Si material have optical gap of 1.89 eV. The efficiency of this single junction solar cell reaches 8.7%. This nc-Si layer can be used not only as an intrinsic layer and as a p-type layer. Also nanocrystalline layer may be used as a seed layer for the growth of polycrystalline Si films at a low temperature.We used single ion beam sputtering methods to synthesize nanocrystalline silicon films successfully. The films were characterized with the technique of X-ray diffraction, Atomic Force Micrographs. We found that the films had a character of nc-amorphous double phase structure. Conductivity test at different temperatures presented the transportation of electrons dominated by different mechanism within different temperature ranges. Photoconductivity gains of the material were obtained in our recent investigation.


2018 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
M.L. Ray ◽  
P.E. Fischione

Abstract Transmission electron microscopy (TEM) specimens are typically prepared using the focused ion beam (FIB) due to its site specificity, and fast and accurate thinning capabilities. However, TEM and high-resolution TEM (HRTEM) analysis may be limited due to the resulting FIB-induced artifacts. This work identifies FIB artifacts and presents the use of argon ion milling for the removal of FIB-induced damage for reproducible TEM specimen preparation of current and future fin field effect transistor (FinFET) technologies. Subsequently, high-quality and electron-transparent TEM specimens of less than 20 nm are obtained.


Author(s):  
H. J. Bender ◽  
R. A. Donaton

Abstract The characteristics of an organic low-k dielectric during investigation by focused ion beam (FIB) are discussed for the different FIB application modes: cross-section imaging, specimen preparation for transmission electron microscopy, and via milling for device modification. It is shown that the material is more stable under the ion beam than under the electron beam in the scanning electron microscope (SEM) or in the transmission electron microscope (TEM). The milling of the material by H2O vapor assistance is strongly enhanced. Also by applying XeF2 etching an enhanced milling rate can be obtained so that both the polymer layer and the intermediate oxides can be etched in a single step.


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.


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