Preparation of thin-film-metal/6H-SiC TEM specimens by RPR ion milling

1993 ◽  
Vol 51 ◽  
pp. 714-715
Author(s):  
J.S. Bow ◽  
F. Shaapur ◽  
M.J. Kim ◽  
R.W. Carpenter
Keyword(s):  
Thin Film ◽  
Good Condition ◽  
Ceramic Materials ◽  
Amorphous Layer ◽  
Thin Metal Film ◽  
Material System ◽  
Ion Milling ◽  
Bonding Structure ◽  
Metal Ceramic ◽  
Milling Method

HRTEM has proven to be the best method to study the interface structure of heterogeneous materials at the atomic level. One of the critical steps in these experiments is preparation of sufficiently thin cross section TEM (XTEM) specimens with different materials on both sides of the interface in good condition for HRTEM, especially when metal/ceramic materials are of interest. For the material system of a thin metal film on 6H-SiC substrate, the conventional ion milling method did not produce satisfactory XTEM specimens, because of the large difference in ion milling rates between metals and SiC. Most of the metal was ion milled way before a thin area of SiC was obtained. Two very important parameters, the thickness of the metal thin film normal to the interface and the atomic bonding structure across the interface were usually lost. Fig.l shows an example. The original thickness of the metal was 100 nm, and most of that has been removed. An amorphous layer of 1 to 1.5 nm thickness apparently due to ion milling formed at the metal/SiC interface.

HREM and AEM study of Pt/SiC interface annealed at high temperature

1993 ◽  
Vol 51 ◽  
pp. 832-833
Author(s):  
J.S. Bow ◽  
L.M. Porter ◽  
M.J. Kim ◽  
R.W. Carpenter ◽  
R.F. Davis
Keyword(s):  
High Temperature ◽  
Image Data ◽  
Amorphous Layer ◽  
Atomic Resolution ◽  
Ceramic Surface ◽  
High Temperature Annealing ◽  
Ion Milling ◽  
Ceramic System ◽  
Residual Oxygen ◽  
Metal Ceramic

High temperature applications of SiC semiconductor devices will be essentially limited by the metal/SiC interface interconnect properties. Pt/SiC was reported to have more stable and better electrical properties than other metal/6H-SiC after annealing above 700°C under UHV condition. Some work on the Pt/SiC interface has been conducted by AES and other low spatial resolution surface techniques, but there is no detailed direct image data reported. Here, we characterize the microstructure of the Pt/SiC interface after high temperature annealing in UHV at near atomic resolution and reported the first nanospectroscopic energy loss data for the system.As-deposited Pt film is polycrystalline with grain size of 10 ± 3 nm (Fig.l). The thin amorphous layer visible at the interface in Fig.l, gradually disappearing in the thick regions, was attributed to oxygen-induced ion-milling damage. Similar results were observed frequently in other metal/ceramic system. We consider the amorphous layer to be due to residual oxygen on the ceramic surface during synthesis, since trace oxygen was only detected at the as-deposited Pt/6H-SiC interface.

Microtomy of spherical Al2O3 powders

1983 ◽  
Vol 41 ◽  
pp. 74-75
Author(s):  
E.J. Jenkins ◽  
D.S. Tucker ◽  
J.J. Hren
Keyword(s):  
Thin Film ◽  
Size Range ◽  
Particle Aggregation ◽  
Ion Milling ◽  
Thin Sections ◽  
Α Phase ◽  
Convenient Means ◽  
Van Der Waals Attraction ◽  
Negative Feature ◽  
Film Substrate

The size range of mineral and ceramic particles of one to a few microns is awkward to prepare for examination by TEM. Electrons can be transmitted through smaller particles directly and larger particles can be thinned by crushing and dispersion onto a substrate or by embedding in a film followed by ion milling. Attempts at dispersion onto a thin film substrate often result in particle aggregation by van der Waals attraction. In the present work we studied 1-10 μm diameter Al2O3 spheres which were transformed from the amprphous state to the stable α phase.After the appropriate heat treatment, the spherical powders were embedded in as high a density as practicable in a hard EPON, and then microtomed into thin sections. There are several advantages to this method. Obviously, this is a rapid and convenient means to study the microstructure of serial slices. EDS, ELS, and diffraction studies are also considerably more informative. Furthermore, confidence in sampling reliability is considerably enhanced. The major negative feature is some distortion of the microstructure inherent to the microtoming operation; however, this appears to have been surprisingly small. The details of the method and some typical results follow.

Microstructural characterization of YBa2Cu3O7-x thin films formed by metalorganic CVD

1991 ◽  
Vol 49 ◽  
pp. 1080-1081
Author(s):  
P. Lu ◽  
W. Huang ◽  
C.S. Chern ◽  
Y.Q. Li ◽  
J. Zhao ◽  
...  
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Critical Current Density ◽  
Critical Current ◽  
Current Density ◽  
Film Growth ◽  
Chemical Vapor ◽  
Microstructural Characterization ◽  
Ion Milling ◽  
Conventional Grinding

The YBa2Cu3O7-x thin films formed by metalorganic chemical vapor deposition(MOCVD) have been reported to have excellent superconducting properties including a sharp zero resistance transition temperature (Tc) of 89 K and a high critical current density of 2.3x106 A/cm2 or higher. The origin of the high critical current in the thin film compared to bulk materials is attributed to its structural properties such as orientation, grain boundaries and defects on the scale of the coherent length. In this report, we present microstructural aspects of the thin films deposited on the (100) LaAlO3 substrate, which process the highest critical current density.Details of the thin film growth process have been reported elsewhere. The thin films were examined in both planar and cross-section view by electron microscopy. TEM sample preparation was carried out using conventional grinding, dimpling and ion milling techniques. Special care was taken to avoid exposure of the thin films to water during the preparation processes.

Stress-Induced Ordering in Y203-Stabilized Tetragonal Zr02

1985 ◽  
Vol 43 ◽  
pp. 222-223
Author(s):  
J. Y. Koo ◽  
M. P. Anderson
Keyword(s):  
Electron Diffraction ◽  
Ionic Conduction ◽  
Electron Diffraction Study ◽  
Ceramic Materials ◽  
Bright Field Image ◽  
Transformation Toughening ◽  
Ion Milling ◽  
Thin Foils ◽  
Carbon Coated ◽  
Convergent Beam

Tetragonal Zr02 has been used as a toughening phase in a large number of ceramic materials. In this system, complex diffraction phenomena have been observed and an understanding of the origin of the diffraction effects provides important information on the nature of transformation toughening, ionic conduction, and phase destabilization. This paper describes the results of an electron diffraction study of Y203-stabilized, tetragonal Zr02 polycrystals (Y-TZP).Thin foils from the bulk Y-TZP sample were prepared by careful grinding and cryo ion-milling. They were carbon coated and examined in a Philips 400T/FEG microscope. Fig. 1 shows a typical bright field image of the 100% tetragonal(t) Zr02. The tetragonal structure was identified by both bulk x-ray diffraction and convergent beam electron diffraction (Fig. 2. A local region within a t-Zr02 grain was subjected to an intense electron beam irradiation which caused partial martensitic transformation of the t-Zr02 to monoclinic(m) symmetry, Fig. 3 A.

Analytical and High-Resolution EM Study of Crystalline Phases formed at Metal-Ceramic Interface

1990 ◽  
Vol 48 (2) ◽  
pp. 426-427
Author(s):  
N. Merk ◽  
A. P. Tomsia ◽  
G. Thomas
Keyword(s):  
Cross Section ◽  
Dissimilar Materials ◽  
Ceramic Materials ◽  
Electron Micrograph ◽  
Scanning Electron Micrograph ◽  
Structural Applications ◽  
Metal Ceramic ◽  
The Subject ◽  
Ceramic Compounds ◽  
Scanning Electron

A recent development of new ceramic materials for structural applications involves the joining of ceramic compounds to metals. Due to the wetting problem, an interlayer material (brazing alloy) is generally used to achieve the bonding. The nature of the interfaces between such dissimilar materials is the subject of intensive studies and is of utmost importance to obtain a controlled microstructure at the discontinuities to satisfy the demanding properties for engineering applications . The brazing alloy is generally ductile and hence, does not readily fracture. It must also wett the ceramic with similar thermal expansion coefficient to avoid large stresses at joints. In the present work we study mullite-molybdenum composites using a brazing alloy for the weldment.A scanning electron micrograph from the cross section of the joining sequence studied here is presented in Fig. 1.

Ion thinning of integrated circuit transverse specimens for transmission electron microscopy

1992 ◽  
Vol 50 (2) ◽  
pp. 1426-1427
Author(s):  
F. Shaapur
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Integrated Circuit ◽  
Substrate Surface ◽  
Homogeneous Material ◽  
Material System ◽  
Ion Milling ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Motion Profile

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.

Microanalysis of silicate glass films grown on α-Al2O3 by pulsed-laser deposition

1993 ◽  
Vol 51 ◽  
pp. 438-439
Author(s):  
Michael P. Mallamaci ◽  
James Bentley ◽  
C. Barry Carter
Keyword(s):  
Liquid Phase ◽  
Single Crystal ◽  
Pulsed Laser Deposition ◽  
Pulsed Laser ◽  
Ceramic Materials ◽  
Laser Deposition ◽  
Triple Junctions ◽  
Ion Milling ◽  
Multicomponent Oxides ◽  
Glass Films

Glass-oxide interfaces play important roles in developing the properties of liquid-phase sintered ceramics and glass-ceramic materials. Deposition of glasses in thin-film form on oxide substrates is a potential way to determine the properties of such interfaces directly. Pulsed-laser deposition (PLD) has been successful in growing stoichiometric thin films of multicomponent oxides. Since traditional glasses are multicomponent oxides, there is the potential for PLD to provide a unique method for growing amorphous coatings on ceramics with precise control of the glass composition. Deposition of an anorthite-based (CaAl2Si2O8) glass on single-crystal α-Al2O3 was chosen as a model system to explore the feasibility of PLD for growing glass layers, since anorthite-based glass films are commonly found in the grain boundaries and triple junctions of liquid-phase sintered α-Al2O3 ceramics.Single-crystal (0001) α-Al2O3 substrates in pre-thinned form were used for film depositions. Prethinned substrates were prepared by polishing the side intended for deposition, then dimpling and polishing the opposite side, and finally ion-milling to perforation.

CBED study of low-temperature InP grown by gas source MBE

1993 ◽  
Vol 51 ◽  
pp. 810-811
Author(s):  
R. Rajesh ◽  
M.J. Kim ◽  
J.S. Bow ◽  
R.W. Carpenter ◽  
G.N. Maracas
Keyword(s):  
Low Temperature ◽  
Second Phase ◽  
Material System ◽  
Ion Milling ◽  
Electrical Measurements ◽  
Gas Source ◽  
Structural And Electrical Properties ◽  
The One ◽  
Lt Inp ◽  
Gas Source Mbe

In our previous work on MBE grown low temperature (LT) InP, attempts had been made to understand the relationships between the structural and electrical properties of this material system. Electrical measurements had established an enhancement of the resistivity of the phosphorus-rich LT InP layers with annealing under a P2 flux, which was directly correlated with the presence of second-phase particles. Further investigations, however, have revealed the presence of two fundamentally different types of precipitates. The first type are the surface particles, essentially an artefact of argon ion milling and containing mostly pure indium. The second type and the one more important to the study are the dense precipitates in the bulk of the annealed layers. These are phosphorus-rich and are believed to contribute to the improvement in the resistivity of the material.The observation of metallic indium islands solely in the annealed LT layers warranted further study in order to better understand the exact reasons for their formation.

Preparation of Ceramic Particulates for Transmission Electron Microscopy

1980 ◽  
Vol 38 ◽  
pp. 196-197
Author(s):  
R. J. Lauf ◽  
H. Keating
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Ceramic Materials ◽  
Ion Milling ◽  
Plastic Films ◽  
Transmission Electron ◽  
Specimen Orientation ◽  
Selection Of

The preparation of fragmented or particulate ceramic materials for transmission electron microscopy (TEM) examination has traditionally been difficult, particularly if a durable, permanent specimen is desired. Furthermore, most established methods for dealing with micron- and submicron-sized samples (e.g., dispersion in plastic films) do not permit selection of orientations or ion thinning. A technique has been developed that is useful for a variety of materials, permits the selection of specimen orientation, is compatible with ion milling requirements, and produces a durable specimen that can be reexamined later if necessary.

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