Microstructural Analysis of Rapid Solidification and Undercooling in the Al-Ge System

1983 ◽  
Vol 28 ◽  
Author(s):  
M.J. Kaufman ◽  
H.L. Fraser
Keyword(s):  
Electron Beam ◽  
Rapid Solidification ◽  
Local Heating ◽  
Microstructural Analysis ◽  
Liquid Droplets ◽  
Amorphous Films ◽  
Phase Selection ◽  
Heating Source ◽  
Electron Microscopes ◽  
Microscope Heating Stage

ABSTRACTSubmicron powders, amorphous films and melt spun ribbons of various Al-Ge alloys have been analyzed to determine the relative roles of undercooling and cooling rate in the production of non-equilibrium structures. All analyses were performed in transmission electron microscopes equipped with energy dispersive x-ray spectrometers. The submicron powders, produced by electro-hydrodynamic atomization, were analyzed in their as-received condition and then annealed and/or melted using the electron beam as a local heating source. Once molten, the liquid droplets were undercooled at different cooling rates by varying the rate of beam obstruction. In this manner, a number of different microstructures were produced. These included metastable crystalline phases and mixed amorphous/crystalline structures. By combining this technique with a microscope heating stage, it was possible to carry out controlled dynamic undercooling experiments and determine phase selection as a function of undercooling and composition. The amorphous films were rapidly heated with the electron beam in the microscope and metastable as well as stable phases were produced. The results of these complementary analyses will be compared and discussed with reference to current models and theories of rapid solidification.

SIZE AND SHAPE MANIPULATION OF SILVER AND INDIUM SMALL PARTICLES BY ELECTRON-BEAM IRRADIATION

1996 ◽  
Vol 03 (01) ◽  
pp. 1113-1119 ◽  
Author(s):  
A. HEILMANN ◽  
A.-D. MÜLLER ◽  
J. WERNER
Keyword(s):  
Electron Beam ◽  
Electron Beam Irradiation ◽  
Local Heating ◽  
Electron Source ◽  
Thin Polymer Film ◽  
Silver Particles ◽  
Beam Irradiation ◽  
Small Particles ◽  
Size And Shape ◽  
Electron Microscopes

Small particles of indium or silver were encapsulated in a thin polymer film matrix by simultaneous plasma polymerization and metal evaporation. Electron-beam irradiation inside transmission electron microscopes and with a microfocus electron source was used to induce changes of the encapsulated particle size and shape. At encapsulated indium particles, substantial microstructural changes were observed during the electron-beam irradiation in the electron microscope. Selected area diffraction demonstrates that indium oxide was formed during the electron irradiation. Additional in situ annealing demonstrates that the indium melting point was not reached during electron-beam-induced local heating of the indium particles. At electron-beam irradiation of plasma polymer films with encapsulated silver particles by using a microfocus electron source, the coalescence of the silver particles can be limited to the irradiated areas of the films.

Modification of the Electron Microscope for Investigation of Fully Hydrated Biological Specimens

1969 ◽  
Vol 27 ◽  
pp. 418-419 ◽  
Author(s):  
R. C. Moretz ◽  
D. F. Parsons
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Structural Damage ◽  
Lower Percentage ◽  
Vacuum Drying ◽  
Total Removal ◽  
Total Absence ◽  
Biological Studies ◽  
Electron Microscopes ◽  
Beam Damage

Short lifetime or total absence of electron diffraction of ordered biological specimens is an indication that the specimen undergoes extensive molecular structural damage in the electron microscope. The specimen damage is due to the interaction of the electron beam (40-100 kV) with the specimen and the total removal of water from the structure by vacuum drying. The lower percentage of inelastic scattering at 1 MeV makes it possible to minimize the beam damage to the specimen. The elimination of vacuum drying by modification of the electron microscope is expected to allow more meaningful investigations of biological specimens at 100 kV until 1 MeV electron microscopes become more readily available. One modification, two-film microchambers, has been explored for both biological and non-biological studies.

Reduction of Specimen Contamination in Electron-Beam Instruments

1976 ◽  
Vol 34 ◽  
pp. 576-577
Author(s):  
G. Lehmpfuhl ◽  
P. J. Smith
Keyword(s):  
Electron Beam ◽  
Cold Trap ◽  
Beam Diameter ◽  
Transmission Electron ◽  
Scanning Transmission ◽  
Hydrocarbon Molecules ◽  
Electron Microscopes ◽  
Combination Of Methods ◽  
Convergent Beam ◽  
Very High

Specimens being observed with electron-beam instruments are subject to contamination, which is due to polymerization of hydrocarbon molecules by the beam. This effect becomes more important as the size of the beam is reduced. In convergent-beam studies with a beam diameter of 100 Å, contamination was observed to grow on samples at very high rates. Within a few seconds needles began forming under the beam on both the top and the underside of the sample, at growth rates of 400-500 Å/s, severely limiting the time available for observation. Such contamination could cause serious difficulty in examining a sample with the new scanning transmission electron microscopes, in which the beam is focused to a few angstroms.We have been able to reduce the rate of contamination buildup by a combination of methods: placing an anticontamination cold trap in the sample region, preheating the sample before observation, and irradiating the sample with a large beam before observing it with a small beam.

A theory of contamination in electron microscopes by surface diffusion

1978 ◽  
Vol 36 (1) ◽  
pp. 116-117
Author(s):  
J.T. Fourie
Keyword(s):  
Electron Beam ◽  
Surface Diffusion ◽  
High Vacuum ◽  
Ultra High Vacuum ◽  
Physical Parameters ◽  
Carbon Compounds ◽  
Hydrocarbon Molecules ◽  
Electron Microscopes ◽  
Primary Electrons ◽  
Long Chain

Contamination in electron microscopes can be a serious problem in STEM or in situations where a number of high resolution micrographs are required of the same area in TEM. In modern instruments the environment around the specimen can be made free of the hydrocarbon molecules, which are responsible for contamination, by means of either ultra-high vacuum or cryo-pumping techniques. However, these techniques are not effective against hydrocarbon molecules adsorbed on the specimen surface before or during its introduction into the microscope. The present paper is concerned with a theory of how certain physical parameters can influence the surface diffusion of these adsorbed molecules into the electron beam where they are deposited in the form of long chain carbon compounds by interaction with the primary electrons.

A New High Intensity Grid Cap for RCA-EMU-3 Electron Microscopes

1968 ◽  
Vol 26 ◽  
pp. 316-317
Author(s):  
George Christov ◽  
Bolivar J. Lloyd
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
High Voltage ◽  
High Intensity ◽  
Electron Gun ◽  
Tungsten Filament ◽  
Fluorescent Screen ◽  
Electron Microscopes ◽  
Pass Through ◽  
Ground Potential

A new high intensity grid cap has been designed for the RCA-EMU-3 electron microscope. Various parameters of the new grid cap were investigated to determine its characteristics. The increase in illumination produced provides ease of focusing on the fluorescent screen at magnifications from 1500 to 50,000 times using an accelerating voltage of 50 KV.The EMU-3 type electron gun assembly consists of a V-shaped tungsten filament for a cathode with a thin metal threaded cathode shield and an anode with a central aperture to permit the beam to course the length of the column. The cathode shield is negatively biased at a potential of several hundred volts with respect to the filament. The electron beam is formed by electrons emitted from the tip of the filament which pass through an aperture of 0.1 inch diameter in the cap and then it is accelerated by the negative high voltage through a 0.625 inch diameter aperture in the anode which is at ground potential.

High-resolution observation of sintered alumina (Al2O3) using the specimen-heated and electron-beam-induced conductivity method in a UHR-SEM

1994 ◽  
Vol 52 ◽  
pp. 1046-1047
Author(s):  
K. Ogura ◽  
T. Suzuki ◽  
C. Nielsen
Keyword(s):  
Electron Beam ◽  
High Resolution ◽  
Specimen Preparation ◽  
Conductivity Method ◽  
Fine Grain ◽  
Grain Structures ◽  
Resolution Observation ◽  
Electron Microscopes ◽  
Scanning Electron Microscopes ◽  
Charging Effect

In spite of the complicated specimen preparation, Transmission Electron Microscopes (TEM) have traditionally been used for the investigation of the fine grain structures of sintered ceramics. Scanning Electron Microscopes (SEM) have not been used much for the same purpose as TEM because of poor results caused by the specimen charging effect, and also the lack of sufficient resolution. Here, we are presenting a successful result of high resolution imaging of sintered alumina (pure Al2O3) using the Specimen Heated and Electron Beam Induced Conductivity (SHEBIC) method, which we recently reported, in an ultrahigh resolution SEM (UHR-SEM). The JSM-6000F, equipped with a Field Emission Gun (FEG) and an in-lens specimen position, was used for this application.After sintered Al2O3 was sliced into a piece approximately 0.5 mm in thickness, one side was mechanically polished to get a shiny plane for the observation. When the observation was started at 20 kV, an enormous charging effect occured, and it was impossible to obtain a clear Secondary Electron (SE) image (Fig.1).

Methods to Monitor and Improve the Performance of Specimen Holders for Transmission Electron Cryomicroscopy

1996 ◽  
Vol 54 ◽  
pp. 454-455
Author(s):  
B. L. Armbruster ◽  
B. Kraus ◽  
M. Pan
Keyword(s):  
Electron Microscopy ◽  
Electron Beam ◽  
Electron Beam Irradiation ◽  
Beam Irradiation ◽  
Quality Of Data ◽  
Electron Cryomicroscopy ◽  
Thermal Equilibration ◽  
Transmission Electron ◽  
Electron Microscopes

One goal in electron microscopy of biological specimens is to improve the quality of data to equal the resolution capabilities of modem transmission electron microscopes. Radiation damage and beam- induced movement caused by charging of the sample, low image contrast at high resolution, and sensitivity to external vibration and drift in side entry specimen holders limit the effective resolution one can achieve. Several methods have been developed to address these limitations: cryomethods are widely employed to preserve and stabilize specimens against some of the adverse effects of the vacuum and electron beam irradiation, spot-scan imaging reduces charging and associated beam-induced movement, and energy-filtered imaging removes the “fog” caused by inelastic scattering of electrons which is particularly pronounced in thick specimens.Although most cryoholders can easily achieve a 3.4Å resolution specification, information perpendicular to the goniometer axis may be degraded due to vibration. Absolute drift after mechanical and thermal equilibration as well as drift after movement of a holder may cause loss of resolution in any direction.

Point-Cathode Electron Gun Using Electron-Beam Bombardment for Cathode Tip Heating

1990 ◽  
Vol 48 (1) ◽  
pp. 198-199
Author(s):  
Ryo Iiyoshi ◽  
Susumu Maruse ◽  
Hideo Takematsu
Keyword(s):  
Electron Beam ◽  
Tungsten Wire ◽  
Local Heating ◽  
Electron Gun ◽  
Original Position ◽  
Beam Power ◽  
Radius Of Curvature ◽  
High Brightness ◽  
Beam Focusing ◽  
Time Operation

Point cathode electron gun with high brightness and long cathode life has been developed. In this gun, a straightened tungsten wire is used as the point cathode, and the tip is locally heated to higher temperatures by electron beam bombardment. The high brightness operation and some findings on the local heating are presented.Gun construction is shown in Fig.l. Small heater assembly (annular electron gun: 5 keV, 1 mA) is set inside the Wehnelt electrode. The heater provides a disk-shaped bombarding electron beam focusing onto the cathode tip. The cathode is the tungsten wire of 0.1 mm in diameter. The tip temperature is raised to the melting point (3,650 K) at the beam power of 5 W, without any serious problem of secondary electrons for the gun operation. Figure 2 shows the cathode after a long time operation at high temperatures, or high brightnesses. Evaporation occurs at the tip, and the tip part retains a conical shape. The cathode can be used for a long period of time. The tip apex keeps the radius of curvature of 0.4 μm at 3,000 K and 0.3 μm at 3,200 K. The gun provides the stable beam up to the brightness of 6.4×106 A/cm2sr (3,150 K) at the accelerating voltage of 50 kV. At 3.4×l06 A/cm2sr (3,040 K), the tip recedes at a slow rate (26 μm/h), so that the effect can be offset by adjusting the Wehnelt bias voltage. The tip temperature is decreased as the tip moves out from the original position, but it can be kept at constant by increasing the bombarding beam power. This way of operation is possible for 10 h. A stepwise movement of the cathode is enough for the subsequent operation. Higher brightness operations with the rapid receding rates of the tip may be improved by a continuous movement of the wire cathode during the operations. Figure 3 shows the relation between the beam brightness, the tip receding rate by evaporation (αis the half-angle of the tip cone), and the cathode life per unit length, as a function of the cathode temperature. The working life of the point cathode is greatly improved by the local heating.

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