Comparison of Ion-Milling Techniques For Cross-Sectional TEM of Semiconductors

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):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


Author(s):  
T. C. Tisone ◽  
S. Lau

In a study of the properties of a Ta-Au metallization system for thin film technology application, the interdiffusion between Ta(bcc)-Au, βTa-Au and Ta2M-Au films was studied. Considered here is a discussion of the use of the transmission electron microscope(TEM) in the identification of phases formed and characterization of the film microstructures before and after annealing.The films were deposited by sputtering onto silicon wafers with 5000 Å of thermally grown oxide. The film thicknesses were 2000 Å of Ta and 2000 Å of Au. Samples for TEM observation were prepared by ultrasonically cutting 3mm disks from the wafers. The disks were first chemically etched from the silicon side using a HNO3 :HF(19:5) solution followed by ion milling to perforation of the Au side.


Author(s):  
C.M. Sung ◽  
M. Levinson ◽  
M. Tabasky ◽  
K. Ostreicher ◽  
B.M. Ditchek

Directionally solidified Si/TaSi2 eutectic composites for the development of electronic devices (e.g. photodiodes and field-emission cathodes) were made using a Czochralski growth technique. High quality epitaxial growth of silicon on the eutectic composite substrates requires a clean silicon substrate surface prior to the growth process. Hence a preepitaxial surface cleaning step is highly desirable. The purpose of this paper is to investigate the effect of surface cleaning methods on the epilayer/substrate interface and the characterization of silicon epilayers grown on Si/TaSi2 substrates by TEM.Wafers were cut normal to the <111> growth axis of the silicon matrix from an approximately 1 cm diameter Si/TaSi2 composite boule. Four pre-treatments were employed to remove native oxide and other contaminants: 1) No treatment, 2) HF only; 3) HC1 only; and 4) both HF and HCl. The cross-sectional specimens for TEM study were prepared by cutting the bulk sample into sheets perpendicular to the TaSi2 fiber axes. The material was then prepared in the usual manner to produce samples having a thickness of 10μm. The final step was ion milling in Ar+ until breakthrough occurred. The TEM samples were then analyzed at 120 keV using the Philips EM400T.


Author(s):  
J.Y. Lee

In the oxidation of metals and alloys, microstructural features at the atomic level play an important role in the nucleation and growth of the oxide, but little is known about the atomic mechanisms of high temperature oxidation. The present paper describes current progress on crystallographic aspects of aluminum oxidation. The 99.999% pure, polycrystalline aluminum was chemically polished and oxidized in 1 atm air at either 550°C or 600°C for times from 0.5 hr to 4 weeks. Cross-sectional specimens were prepared by forming a sandwich with epoxy, followed by mechanical polishing and then argon ion milling. High resolution images were recorded in a <110>oxide zone-axis orientation with a JE0L JEM 200CX microscope operated at 200 keV.


Author(s):  
F. Shaapur

Non-uniform ion-thinning of heterogenous material structures has constituted a fundamental difficulty in preparation of specimens for transmission electron microscopy (TEM). A variety of corrective procedures have been developed and reported for reducing or eliminating the effect. Some of these techniques are applicable to any non-homogeneous material system and others only to unidirectionalfy heterogeneous samples. Recently, a procedure of the latter type has been developed which is mainly based on a new motion profile for the specimen rotation during ion-milling. This motion profile consists of reversing partial revolutions (RPR) within a fixed sector which is centered around a direction perpendicular to the specimen heterogeneity axis. The ion-milling results obtained through this technique, as studied on a number of thin film cross-sectional TEM (XTEM) specimens, have proved to be superior to those produced via other procedures.XTEM specimens from integrated circuit (IC) devices essentially form a complex unidirectional nonhomogeneous structure. The presence of a variety of mostly lateral features at different levels along the substrate surface (consisting of conductors, semiconductors, and insulators) generally cause non-uniform results if ion-thinned conventionally.


Author(s):  
H. Takaoka ◽  
M. Tomita ◽  
T. Hayashi

High resolution transmission electron microscopy (HRTEM) is the effective technique for characterization of detailed structure of semiconductor materials. Oxygen is one of the important impurities in semiconductors. Detailed structure of highly oxygen doped silicon has not clearly investigated yet. This report describes detailed structure of highly oxygen doped silicon observed by HRTEM. Both samples prepared by Molecular beam epitaxy (MBE) and ion implantation were observed to investigate effects of oxygen concentration and doping methods to the crystal structure.The observed oxygen doped samples were prepared by MBE method in oxygen environment on (111) substrates. Oxygen concentration was about 1021 atoms/cm3. Another sample was silicon of (100) orientation implanted with oxygen ions at an energy of 180 keV. Oxygen concentration of this sample was about 1020 atoms/cm3 Cross-sectional specimens of (011) orientation were prepared by argon ion thinning and were observed by TEM at an accelerating voltage of 400 kV.


1994 ◽  
Vol 357 ◽  
Author(s):  
A. J. Pedraza ◽  
Siqi Cao ◽  
L. F. Allard ◽  
D. H. Lowndes

AbstractA near-surface thin layer is melted when single crystal alumina (sapphire) is pulsed laserirradiated in an Ar-4%H2 atmosphere. γ-alumina grows epitaxially from the (0001) face of axalumina (sapphire) during the rapid solidification of this layer that occurs once the laser pulse is over. Cross sectional high resolution transmission electron microscopy (HRTEM) reveals that the interface between unmelted sapphire and γ-alumina is atomistically flat with steps of one to a few close-packed oxygen layers; however, pronounced lattice distortions exist in the resolidified γ-alumina. HRTEM also is used to study the metal-ceramic interface of a copper film deposited on a laser-irradiated alumina substrate. The observed changes of the interfacial structure relative to that of unexposed substrates are correlated with the strong enhancement of film-substrate bonding promoted by laser irradiation. HRTEM shows that a thin amorphous film is produced after irradiation of 99.6% polycrystalline alumina. Formation of a diffuse interface and atomic rearrangements that can take place in metastable phases contribute to enhance the bonding strength of copper to laser-irradiated alumina.


1992 ◽  
Vol 7 (8) ◽  
pp. 2225-2229 ◽  
Author(s):  
Z.G. Li ◽  
P.F. Carcia ◽  
P.C. Donohue

The microstructure of LaB6-base thick film resistors was investigated by cross-sectional transmission electron microscopy. The specimens were prepared by a technique that polished them to a thin wedge, thus avoiding ion-milling and permitting imaging over a distance of tens of microns. The resistor microstructure contained a finely divided electrically conductive phase of TaB2 and nonconducting crystals of CaTa4O11, formed during high temperature processing of glass and LaB6 ingredients of the thick film ink. Using higher surface area ingredients virtually suppressed the formation of CaTa4O11 crystals, and the microstructure became more uniform. Resistors made with higher surface area intermediates also had better voltage withstanding properties.


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