In Situ Observation of Catalyzed Gasification of Graphite by Nickel

Author(s):  
R. T. K. Baker ◽  
R. D. Sherwood

The catalytic gasification of carbon at high temperature by microscopic size metal particles is of fundamental importance to removal of coke deposits and conversion of refractory hydrocarbons into fuels and chemicals. The reaction of metal/carbon/gas systems can be observed by controlled atmosphere electron microscopy (CAEM) in an 100 KV conventional transmission microscope. In the JEOL gas reaction stage model AGl (Fig. 1) the specimen is positioned over a hole, 200μm diameter, in a platinum heater strip, and is interposed between two apertures, 75μm diameter. The control gas flows across the specimen and exits through these apertures into the specimen chamber. The gas is further confined by two apertures, one in the condenser and one in the objective lens pole pieces, and removed by an auxiliary vacuum pump. The reaction zone is <1 mm thick and is maintained at gas pressure up to 400 Torr and temperature up to 1300<C as measured by a Pt-Pt/Rh 13% thermocouple. Reaction events are observed and recorded on videotape by using a Philips phosphor-television camera located below a hole in the center of the viewing screen. The overall resolution is greater than 2.5 nm.

Author(s):  
William Krakow

An electronic device has been constructed which manipulates the primary beam in the conventional transmission microscope to illuminate a specimen under a variety of virtual condenser aperture conditions. The device uses the existing tilt coils of the microscope, and modulates the D.C. signals to both x and y tilt directions simultaneously with various waveforms to produce Lissajous figures in the back-focal plane of the objective lens. Electron diffraction patterns can be recorded which reflect the manner in which the direct beam is tilted during exposure of a micrograph. The device has been utilized mainly for the hollow cone imaging mode where the device provides a microscope transfer function without zeros in all spatial directions and has produced high resolution images which are also free from the effect of chromatic aberration. A standard second condenser aperture is employed and the width of the cone annulus is readily controlled by defocusing the second condenser lens.


Author(s):  
A. V. Crewe ◽  
M. W. Retsky

A 100 kv scanning transmission microscope has been built. Briefly, the design is as follows: The electron gun consists of a field emission point and a 3 cm Butler gun. The beam has a crossover outside the gun and is collimated by a condenser lens.The parallel beam passes through a defining aperture and is focused by the objective lens onto the specimen. The elastic electrons are detected by two annular detectors, each subtending a different angle, and the unscattered and inelastic electrons are collected by a third detector. The spectrometer that will separate the inelastic and unscattered electrons has not yet been built.The lens current supplies are stable to within one part per million per hour and have been described elsewhere.The high voltage is also stable to 1 ppm/hr. It consists of the raw supply from a 100 kv Spellman power supply controlled by an external reference voltage, high voltage divider, and error amplifier.


Author(s):  
R-R. Lee

Partially-stabilized ZrO2 (PSZ) ceramics have considerable potential for advanced structural applications because of their high strength and toughness. These properties derive from small tetragonal ZrO2 (t-ZrO2) precipitates in a cubic (c) ZrO2 matrix, which transform martensitically to monoclinic (m) symmetry under applied stresses. The kinetics of the martensitic transformation is believed to be nucleation controlled and the nucleation is always stress induced. In situ observation of the martensitic transformation using transmission electron microscopy provides considerable information about the nucleation and growth aspects of the transformation.


Author(s):  
S. Hagège ◽  
U. Dahmen ◽  
E. Johnson ◽  
A. Johansen ◽  
V.S. Tuboltsev

Small particles of a low-melting phase embedded in a solid matrix with a higher melting point offer the possibility of studying the mechanisms of melting and solidification directly by in-situ observation in a transmission electron microscope. Previous studies of Pb, Cd and other low-melting inclusions embedded in an Al matrix have shown well-defined orientation relationships, strongly faceted shapes, and an unusual size-dependent superheating before melting.[e.g. 1,2].In the present study we have examined the shapes and thermal behavior of eutectic Pb-Cd inclusions in Al. Pb and Cd form a simple eutectic system with each other, but both elements are insoluble in solid Al. Ternary alloys of Al (Pb,Cd) were prepared from high purity elements by melt spinning or by sequential ion implantation of the two alloying additions to achieve a total alloying addition of up to lat%. TEM observations were made using a heating stage in a 200kV electron microscope equipped with a video system for recording dynamic behavior.


Author(s):  
K. Fukushima ◽  
N. Kohyama ◽  
A. Fukami

A film-sealed high resolution environmental cell(E.C) for observing hydrated materials had been developed by us(l). Main specification of the E.C. is as follows: 1) Accelerated voltage; 100 kV. 2) Gas in the E.C.; saturated water vapour with carrier gas of 50 Torr. 3) Thickness of gas layer; 50 μm. 4) Sealing film; evaporated carbon film(20 nm thick) with plastic microgrid. 5) Resolving power; 1 nm. 6) Transmittance of electron beam; 60% at 100 kV. The E.C. had been successfully applied to the study of hydrated halloysite(2) (3). Kaolin minerals have no interlayer water and are basically non-expandable but form intercalation compounds with some specific chemicals such as hydrazine, formamide and etc. Because of these compounds being mostly changed in vacuum, we tried to reveal the structure changes between in wet air and in vacuum of kaolin minerals intercalated with hydrazine and of hydrated state of montmori1lonite using the E.C. developed by us.


2013 ◽  
Vol 133 (12) ◽  
pp. 350-357
Author(s):  
Yuta Nakashima ◽  
Ryo Monji ◽  
Katsuya Sato ◽  
Kazuyuki Minami

2012 ◽  
Vol 19 (3) ◽  
pp. 583-592 ◽  
Author(s):  
Yinke Dou ◽  
Xiaomin Chang

Abstract Ice thickness is one of the most critical physical indicators in the ice science and engineering. It is therefore very necessary to develop in-situ automatic observation technologies of ice thickness. This paper proposes the principle of three new technologies of in-situ automatic observations of sea ice thickness and provides the findings of laboratory applications. The results show that the in-situ observation accuracy of the monitor apparatus based on the Magnetostrictive Delay Line (MDL) principle can reach ±2 mm, which has solved the “bottleneck” problem of restricting the fine development of a sea ice thermodynamic model, and the resistance accuracy of monitor apparatus with temperature gradient can reach the centimeter level and research the ice and snow substance balance by automatically measuring the glacier surface ice and snow change. The measurement accuracy of the capacitive sensor for ice thickness can also reach ±4 mm and the capacitive sensor is of the potential for automatic monitoring the water level under the ice and the ice formation and development process in water. Such three new technologies can meet different needs of fixed-point ice thickness observation and realize the simultaneous measurement in order to accurately judge the ice thickness.


2020 ◽  
Vol 13 (10) ◽  
pp. 105501
Author(s):  
Kuan-Kan Hu ◽  
Kensaku Maeda ◽  
Keiji Shiga ◽  
Haruhiko Morito ◽  
Kozo Fujiwara

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