Sample Preparation of Al-Alloys for 3D FIB Nano-Characterization

AbstractAs a preliminary step to detailed study of the interfaces in SiC particulatereinforced Al alloys, a number of methods of sample preparation have been explored; the resultant artefacts on the thinned foils observed in transmission electron microscopes are discussed and improvements to the preparation procedures are suggested. Initial observations of the microstructure of two alloys differing significantly in their matrix silicon content are presented.

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Pollutant Identification by Selected Area Electron Diffraction

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100052675 ◽

1974 ◽

Vol 32 ◽

pp. 532-533

Author(s):

R. E. Ferrell ◽

G. G. Paulson ◽

C. W. Walker

Keyword(s):

Thermal Treatment ◽

Electron Diffraction ◽

Sample Preparation ◽

Crystal Structures ◽

Water Samples ◽

Environmental Samples ◽

Short Review ◽

Selected Area Electron Diffraction ◽

Multiple Component

Selected area electron diffraction (SAD) has been used successfully to determine crystal structures, identify traces of minerals in rocks, and characterize the phases formed during thermal treatment of micron-sized particles. There is an increased interest in the method because it has the potential capability of identifying micron-sized pollutants in air and water samples. This paper is a short review of the theory behind SAD and a discussion of the sample preparation employed for the analysis of multiple component environmental samples.

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Preparation of Thin Cadmium Telluride Samples for Electron Microscope Studies

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100052754 ◽

1974 ◽

Vol 32 ◽

pp. 548-549

Author(s):

T. J. Magee ◽

J. Peng ◽

J. Bean

Keyword(s):

Electron Microscope ◽

Sulfuric Acid ◽

Solid State ◽

Sample Preparation ◽

Cadmium Telluride ◽

Potassium Dichromate ◽

Optical Components ◽

The Past ◽

Solid State Devices

Cadmium telluride has become increasingly important in a number of technological applications, particularly in the area of laser-optical components and solid state devices, Microstructural characterizations of the material have in the past been somewhat limited because of the lack of suitable sample preparation and thinning techniques. Utilizing a modified jet thinning apparatus and a potassium dichromate-sulfuric acid thinning solution, a procedure has now been developed for obtaining thin contamination-free samples for TEM examination.

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A Freeze Shadow Technique for the Preparation of Soft Paint Latexes for Electron Microscopy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100079097 ◽

1977 ◽

Vol 35 ◽

pp. 314-315

Author(s):

Earl R. Walter ◽

Glen H. Bryant

Keyword(s):

Sample Preparation ◽

High Vacuum ◽

Vacuum System ◽

Latex Particles ◽

New Methods ◽

Diffusion Pump ◽

Film Forming ◽

Routine Basis ◽

Distribution Studies ◽

Preparation Techniques

With the development of soft, film forming latexes for use in paints and other coatings applications, it became desirable to develop new methods of sample preparation for latex particle size distribution studies with the electron microscope. Conventional latex sample preparation techniques were inadequate due to the pronounced tendency of these new soft latex particles to distort, flatten and fuse on the substrate when they dried. In order to avoid these complications and obtain electron micrographs of undistorted latex particles of soft resins, a freeze-dry, cold shadowing technique was developed. The method has now been used in our laboratory on a routine basis for several years.The cold shadowing is done in a specially constructed vacuum system, having a conventional mechanical fore pump and oil diffusion pump supplying vacuum. The system incorporates bellows type high vacuum valves to permit a prepump cycle and opening of the shadowing chamber without shutting down the oil diffusion pump. A baffeled sorption trap isolates the shadowing chamber from the pumps.

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SEM evaluation of the TEM cold-stage double-film specimen

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100111471 ◽

1984 ◽

Vol 42 ◽

pp. 272-273

Author(s):

Jayesh Bellare

Keyword(s):

Spatial Distribution ◽

Sample Preparation ◽

Sample Thickness ◽

Specimen Preparation ◽

Preparation Technique ◽

Liquid Sample ◽

Thin Specimen ◽

Sample Preparation Technique ◽

Cold Stage ◽

Film Specimen

Seeing is believing, but only after the sample preparation technique has received a systematic study and a full record is made of the treatment the sample gets.For microstructured liquids and suspensions, fast-freeze thermal fixation and cold-stage microscopy is perhaps the least artifact-laden technique. In the double-film specimen preparation technique, a layer of liquid sample is trapped between 100- and 400-mesh polymer (polyimide, PI) coated grids. Blotting against filter paper drains excess liquid and provides a thin specimen, which is fast-frozen by plunging into liquid nitrogen. This frozen sandwich (Fig. 1) is mounted in a cooling holder and viewed in TEM.Though extremely promising for visualization of liquid microstructures, this double-film technique suffers from a) ireproducibility and nonuniformity of sample thickness, b) low yield of imageable grid squares and c) nonuniform spatial distribution of particulates, which results in fewer being imaged.

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Observation of faint contrast at planar faults in alloys

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100108842 ◽

1978 ◽

Vol 36 (1) ◽

pp. 340-341

Author(s):

K. Kuroda ◽

Y. Tomokiyo ◽

T. Kumano ◽

T. Eguchi

Keyword(s):

Reciprocal Lattice ◽

Beam Theory ◽

Al Alloys ◽

Small Displacement ◽

Electron Microscopic ◽

Lattice Vector ◽

Fringe Contrast ◽

Planar Fault ◽

Lattice Displacement ◽

The Many

The contrast in electron microscopic images of planar faults in a crystal is characterized by a phase factor , where is the reciprocal lattice vector of the operating reflection, and the lattice displacement due to the fault under consideration. Within the two-beam theory a planar fault with an integer value of is invisible, but a detectable contrast is expected when the many-beam dynamical effect is not negligibly small. A weak fringe contrast is also expected when differs slightly from an integer owing to an additional small displacement of the lattice across the fault. These faint contrasts are termed as many-beam contrasts in the former case, and as ε fringe contrasts in the latter. In the present work stacking faults in Cu-Al alloys and antiphase boundaries (APB) in CuZn, FeCo and Fe-Al alloys were observed under such conditions as mentioned above, and the results were compared with the image profiles of the faults calculated in the systematic ten-beam approximation.

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Advanced TEM sample preparation techniques for submicron Si devices

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100138956 ◽

1995 ◽

Vol 53 ◽

pp. 516-517 ◽

Cited By ~ 1

Author(s):

P. B. Basham ◽

H. L. Tsai

Keyword(s):

Sample Preparation ◽

Process Development ◽

Light Transmission ◽

Specific Area ◽

Turnaround Time ◽

Small Hole ◽

Area Of Interest ◽

Transmission Electron ◽

Polished Side ◽

Preparation Techniques

The use of transmission electron microscopy (TEM) to support process development of advanced microelectronic devices is often challenged by a large amount of samples submitted from wafer fabrication areas and specific-spot analysis. Improving the TEM sample preparation techniques for a fast turnaround time is critical in order to provide a timely support for customers and improve the utilization of TEM. For the specific-area sample preparation, a technique which can be easily prepared with the least amount of effort is preferred. For these reasons, we have developed several techniques which have greatly facilitated the TEM sample preparation.For specific-area analysis, the use of a copper grid with a small hole is found to be very useful. With this small-hole grid technique, TEM sample preparation can be proceeded by well-established conventional methods. The sample is first polished to the area of interest, which is then carefully positioned inside the hole. This polished side is placed against the grid by epoxy Fig. 1 is an optical image of a TEM cross-section after dimpling to light transmission.

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Quantitative defect studies in semiconductor TEM samples prepared by low angle ion milling

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100138932 ◽

1995 ◽

Vol 53 ◽

pp. 512-513

Author(s):

L. Mulestagno ◽

J.C. Holzer ◽

P. Fraundorf

Keyword(s):

Sample Preparation ◽

Milling Time ◽

High Density ◽

Low Density ◽

Ion Milling ◽

High Quality ◽

Variable Angle ◽

Major Disadvantage ◽

Induced Defects

Due to the wealth of information, both analytical and structural that can be obtained from it TEM always has been a favorite tool for the analysis of process-induced defects in semiconductor wafers. The only major disadvantage has always been, that the volume under study in the TEM is relatively small, making it difficult to locate low density defects, and sample preparation is a somewhat lengthy procedure. This problem has been somewhat alleviated by the availability of efficient low angle milling.Using a PIPS® variable angle ion -mill, manufactured by Gatan, we have been consistently obtaining planar specimens with a high quality thin area in excess of 5 × 104 μm2 in about half an hour (milling time), which has made it possible to locate defects at lower densities, or, for defects of relatively high density, obtain information which is statistically more significant (table 1).

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Microstructure of an extruded rapidly solidified Al-8Fe-2Mo alloy

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100144218 ◽

1986 ◽

Vol 44 ◽

pp. 548-549

Author(s):

W. T. Donlon ◽

J. E. Allison ◽

S. Shinozaki

Keyword(s):

Electron Microscopy ◽

Automotive Industry ◽

Fuel Economy ◽

High Strength ◽

Al Alloys ◽

Light Weight ◽

Thin Sections ◽

Strength And Durability ◽

Rapidly Solidified ◽

Whitney Aircraft

Light weight materials which possess high strength and durability are being utilized by the automotive industry to increase fuel economy. Rapidly solidified (RS) Al alloys are currently being extensively studied for this purpose. In this investigation the microstructure of an extruded Al-8Fe-2Mo alloy, produced by Pratt & Whitney Aircraft, Goverment Products Div. was examined in a JE0L 2000FX AEM. Both electropolished thin sections, and extraction replicas were examined to characterize this material. The consolidation procedure for producing this material included a 9:1 extrusion at 340°C followed by a 16:1 extrusion at 400°C, utilizing RS powders which have also been characterized utilizing electron microscopy.

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